Sassafras is fascinating. Bill and I compared notes. We had each looked at the web sites of botanical gardens and arboretums, finding specimens, listings, and descriptions.
There’s a good YouTube video on harvesting sapling roots for root beer (sure!). Some herb and spice places sell the dried root; it’s even available via Amazon.com. A cool fact is that Atlanta volunteers planted 200 sassafras trees along a section of the Beltline trail system. It was Georgia’s Plant of the Year some years ago.
Sassafras trees produce safrole, a root beer – smelling oil with a fascinating, and complex, chemical structure. From pure safrole it’s only a few chemical steps to MDMA. There are some trees and shrubs with very high safrole contents, especially in certain areas of the tropics.
The rain forests in the Cardamom Mountains of Cambodia were being destroyed by the harvesting of Cinnamomum parthenoxylon trees for sassafras oil, which is shipped to Europe and Asia for MDMA synthesis. The issue is covered in Drugs Unlimited, by Mike Power, and documented in a 20 minute film titled Forest of Ecstasy.
We learned there’s an herb and tea supplier in Watsonville, California that sells sassafras root bark for $35 per pound. I bought some online.
Tom and I discussed synthesis routes and final chemical needs. He was preparing to return to Oregon in a few days and spend two weeks setting up and testing the lab between his chemo treatments. Peter and Lucien were cleaning up and furnishing the place in preparation for his return.
“Are we staying focused on MDMA?” Tom asked.
“Yes,” I answered.
“I thought there was some other agents, more effective for revelation purposes than LSD or MDMA,” Tom said.
“Nothing as good as MDMA. Power discusses, in Drugs Unlimited, an interesting variant called 6-APB – it’s essentially MDMA with one of the dioxygen ring’s hydrogens missing. He quoted an English major Jeffrey Jenkins as saying
MDMA intrigued me .. with its strangely universal experience, its ability to make even the hardest soul empathic….
“An English major!” Tom said. “He didn’t make the stuff, did he?”
“Sorry to bust your expertise bubble,” I smiled, “but Jenkins apparently taught himself organic chemistry so he could make his own MDMA – and then legal variants – and he put it all online. Although 6-APB was formally legal in Britain, they busted him and jailed him anyway.”
“‘Make even the hardest soul empathic’… I love that. Weren’t there earlier attempts at something better – even by Shulgin?” Tom asked.
“Yes, but I think Sasha and Ann both agreed they never experienced anything better than MDMA. There was a lot of interest – and much effort by the CIA and the Army – way back,” I said. “Much of the history is in the Acid Dreams book of 1985, just before MDMA became widely known.”
We were now back in Oregon, setting up the lab.
Some homework revealed that there were several so-called super-hallucinogens studied by the Army and the CIA in the sixties and seventies. The most developed and tested was BZ – Army code EA2277. In addition to the Acid Dreams book, which relied on declassified Army and CIA files, there was a mea culpa book by an Army Chemical Warfare Colonel, James Ketchum, published in 2006: Chemical Warfare: Secrets Almost Forgotten. The New Yorker discussed Ketchum and his book in a December 2012 piece (just after the paperback version was published) called Operation Delirium. Much of the Army work was on aerosol delivery – sort of a psychic gas approach.
“Cool!” Lucien said. “That must be what stimulated a Sherlock TV episode that used a military psycho-chemical gas – The Hound of the Baskervilles. I saw it a few weeks ago via Netflix.”
“So the Army wanted to use gas or aerosol delivery?” Tom asked.
“Yes. But for military – not political revelation – purposes, although many of the LSD pioneers had ideas about political and cultural transformation via LSD – Hubbard, Osmond, Kesey, Leary – and others,” I said.
“And funded by the Army and the CIA,” Lucien said. “In the Sherlock episode – I think it was in Season 2, it was to cause delirium and total incapacitation.”
“How much TV do you watch,” I joked.
“When you’re 44, single, and without much social life, Sherlock helps.”
“Do see, if you haven’t, Cumberbatch’s The Imitation Game,” Tom suggested. “He’s not only a great Sherlock, but also a great Alan Turing.”
I continued: “BZ was intensively studied and tested over a two week period at Utah’s Dugway Proving Grounds – at least according to Ketchum’s book. The project was unofficially called Project Dork – a play on the ‘crazy’ General Dick who ordered the test. BZ was likely burned and eliminated there later at the Army’s Chemical Agent Disposal Facility nearby.”
“It seems there’s always some Utah connection,” Lucien noted.
“Well, BZ is not a psychedelic and was not studied by Shulgin – although, interestingly, he wrote a brief Preface for Ketchum’s book. BZ can be considered an incapacitating agent. Shulgin called it a ‘deleriant’ on p. 218 of The Shulgin Index.”
Project MK-Ultra was an even earlier government ‘research’ effort, from about 1953 to 1973, by the CIA and the Army, to apply methodologies to manipulate people’s mental states and alter their brain functions. The goal was to develop truth-telling capabilities, often involving the surreptitious administration of LSD or other drugs. Research was done at some 80 institutions, including colleges and universities, hospitals, prisons and pharmaceutical companies in the US and Canada. The CIA used various front organizations to fund and monitor the work. In many respects the CIA was thus responsible for the ready availability of LSD among the research and medical communities. The program was made public via the Church Committee investigations stemming from FBI surveillance activities, chronicled in the recent documentary 1971.
There’s been some interest in methylone, sometimes considered a substitute for MDMA. A Breaking Bad – like Chinese professor, a Dr. Zhang, set up a lab and, in 2014, before he was caught, sold methylone. It’s essentially a ketone derivative of MDMA. Perhaps he chose it because he thought it was outside of Chinese or Australian drug laws. It was available in The Netherlands in 2004 under the street name Explosion.
Shulgin also made and evaluated methylone, saying it
…has almost the same potency, but it doesn’t produce the same effects. It has an almost antidepressant action, pleasant and positive, but not the unique magic of MDMA.
In addition to all the positive experiences with MDMA over the years, Shulgin’s review in PIHKAL is among the best:
I feel absolutely clean inside, and there is nothing but pure euphoria. I have never felt so great, or believed this to be possible. The cleanliness, clarity, and marvelous feeling of solid inner strength continued through the rest of the day, and evening, and into the next day. I am overcome by the profundity of the experience…
“MDMA has most of the effects we want – ” said Peter, “- decreased personal fear of others and of the unknown, decreased social anxiety, increased empathy, general openness and wellbeing, and for most a real personal transformation, revelation.”
“And since we will likely have only one major opportunity to use it on each of our patients, I think we’ll want to use at least 100 mg amounts – perhaps 125 mg for big people,” I said.
“Shulgin’s 1986 paper is the best synthesis summary I’ve seen – six routes to MDMA,” said Tom.
“Yes,” I agreed. “He also published one that same year on his testing protocol for new drugs, via self-experimentation – the Shulgin Protocol.”
“As one of the key testers, I’m pleased to learn there’s a protocol,” Lucien added.
I continued: “The more recent papers from the forensic communities have been very helpful – they tend to focus on impurities in the various synthetic processes, with the goal of helping to identify clandestine labs.”
“My thought is that the original safrole bromination process is the most direct, involves fewer chemicals, and results in a less traceable MDMA product,” Tom continued. “That route doesn’t involve MDA, a common contaminant of clandestine MDMA.”
“It’s just two steps, isn’t it?” I asked.
“Yes – by brominating safrole’s propylene group, followed by a methylamine replacement of the bromine,” Tom said. “The reaction’s been studied by the Polish forensics community; the more recent papers are readily available in English.”
“So we only need hydrobromic acid and methylamine? And the safrole?”
“A steam extraction and distillation gets us safrole from sassafras,” Tom continued. “You know, it’s curious that Shulgin doesn’t mention the direct safrole to MDMA route in PIHKAL, but includes it in The Shulgin Index, published in 2011, some 20 years later.”
“MDMA merits the longest discussion in the Index, but with no synthesis details – lots on analytical chemistry, however. It’s been noted that the bromo approach produces relatively low yields compared to other routes, which is probably why Shulgin didn’t use it much,” I said.
“Increasing the yield involves using a high pressure reaction step which isn’t difficult. If we were into making large amounts of MDMA, we’d consider it,” Tom added.
“We need to do much more homework focused on potential side reactions and impurities – and on various purification steps and procedures,” I said. “ – and on analytical methods.”
“Agreed,” Tom concluded.
We already know that MDMA is an incredible molecule. It’s chemical structure suggests amphetamine, met-amphetamine, MDA, and something else – all rolled into one very special molecule that is non-addictive, non-hallucinogenic, non-toxic; no visions, no crazy images – just a gentle, open, relaxed, empathogenic frame of mind. Huxley would have loved it. Of all the ‘psychedelics’, it’s the closest to his ideal moksha, described in his final novel, Island. And not at all like the soma of his Brave New World – and not at all like LSD.
“Huxley started with mescaline, got to LSD via Osmond, and experienced psilocybin via his work with Timothy Leary. MDMA didn’t become available until the early eighties, some 20 years after Huxley died,” Peter said.
“I’m now reading Moksha, a collection of his shorter writings – letters, speeches from 1931 through 1963.” I said. “I started with the most recent, working back in time. What a wonderful, perceptive, open thinker and writer. He foresaw and cautioned us against almost everything we are now concerned about in our modern overpopulated, over consumptive, over technological, and over politicized society.”
“Amen,” Tom said.
I planned to acquire multiple small bottles of the solvents and reagents needed for all major MDMA synthesis pathways, in case the direct safrole to MDMA bromine-based reaction isn’t adequate for our needs. This would be done in stages from different sources: borrowing small amounts, getting some from the U Chemistry stockroom, and independent orders from the major chemical suppliers – spread over several months. As methylamine is a ‘watched’ substance, I will ‘borrow’ it from some chemistry researcher friends. We can also directly synthesize it.
The bromination – methylamine route is simple and direct, although there have been reports of low yields. That’s not a problem as long as we are careful to purify the MDMA and as long as any residual impurities are not particularly toxic. Clandestine street products are rarely carefully purified or characterized – and it’s those products to which the forensic labs and ‘watchers’ are tuned or focused. The bromination route of course has the major advantage that we can start from sassafras. Although it, too, is likely ‘watched’, especially safrole oil, we will obtain sassafras in small quantities from multiple sources, ostensibly for botanical studies and for root beer and tea preparation.
It’s interesting that Shulgin’s procedures required long times – much patience. He originally used the slower, safer processes. He was also very concerned with purification and characterization. Time and patience are not normal characteristics of clandestine drug synthesizers or dealers.
The drug forensics people have provided detailed information on synthesis via the various routes. They do that to understand the various impurities so as to try to identify labs of origin for street drugs. The forensics papers are the most helpful for harmless!
“Hydrobromic acid is nasty stuff,” I said to Tom.
“Most strong acids are,” he responded. “We chemists understand and respect acids. HBr is a stronger acid than hydrochloric but no more difficult to work with. We’ll just use a good chemical hood and ventilation. Not to worry.”
“I’m more concerned about that,” Tom answered. “Maybe I’ve watched too many Breaking Bad! episodes. Since methylamine is a key ingredient in meth labs, it’s likely to be ‘watched’ much more that sassafras or safrole. I’ll need to use a respirator mask and good ventilation. But that’s standard for real organic chemists.”
“You’re the chemist,” I said.
The demand for MDMA is high. About 25,000 kg are used yearly in Britain, most of it coming from Holland via land, air and sea. Each kilo of MDMA costs about $1,000 to produce, but is sold wholesale for about $4,000. Middlemen pay about $15,000/kilo. A gram on the streets costs up to $50 – that would be up to 10 doses of pure MDMA.
I obtained some methylamine solution from a friend who was retiring and cleaning out her lab. No methylamine paper trails. Hydrobromic acid, 48%, I purchased from the U Chemistry stockroom, and bought sassafras root and bark from several different tea and herb sources online.
I checked out the vacuum pump and the various lab equipment obtained from the stockroom and from Surplus and Salvage. The small, portable fume hood worked fine. I bought a venting hose from Home Depot. This was all to go to Tom’s new home and lab in Portland.
But we did need more glassware and equipment: a rotary evaporator, better funnels, heating mantles, thermometers, a manometer for vacuum distillations, and several more ice/cooling baths. Back to Surplus and Salvage.
The TLC plates and developing equipment are also going to Portland. We will also experiment with some high performance TLC methods to hopefully improve the TLC analysis and detection.
I considered keeping the Raman spectrometer in my U office, to help provide credibility for my purchases and new research project, but in the end decided it, too, needed to be in Portland so we could perform all the analyses there. With my earlier Raman collaborator, we modified the software to make it easier to use for our harmless needs. I also purchased the silver colloid precursors to facilitate the SERS analysis.
We scheduled our trip. Tom will fly again to Portland next weekend. I’ll drive by way of Winnemucca and Denio Junction; I just love that long, lonely road through NW Nevada.
By then Lucien and Peter will have the Portland house in shape, with the new locks and appropriate lights and fans for our needs. Tom decided to set up the ‘lab’ in the basement half-bath (just basin and toilet); it does have a basement window suitable for hood venting; there are other basement windows to facilitate air movement via fans. Lucien’s already planted small bushes and grasses outside the basement windows to increase basement privacy. Much of the work will be done during daylight times to avoid need for nighttime basement lights. As we get started we’ll monitor any odors or other signals which might lead anyone on the street to ask what’s going on (lots of people have watched Breaking Bad!).
Diana and I drove to Portland via I-80, Denio Junction, and I-5. She agreed to come along to spend a few days with her sisters in Portland.
Our no longer pristine Prius had several small boxes of chemicals – for, if asked, chemistry and luminescence demonstrations I arranged to do at a small science center in Eugene. I also do Leonardo da Vinci ‘shows’ for classes and science centers. These have been serious education outreach activities for me, but now they provide cover for harmless. Diana and I also carried small equipment, the Raman system, the portable hood, and my Leonardo posters and gear, as well as our travel suitcases.
The chemicals and solvents were, of course, ‘mis’-labeled in accordance with what I’d be doing in the demonstrations and shows. Given the chemical sophistication of our population, I didn’t expect any problems.
We got to Portland and unloaded without any questions or issues. Diana spent the next several days mainly with her sisters. Tom and I, together with Peter and Lucien, moved into Tom’s new home – the harmless cottage – and began to set up shop.
We used an old, used refrigerator as the basement chemical storage safety cabinet. We set up a sturdy used table right outside the downstairs bathroom, placed the portable hood on it, ran the vent to the basement window behind some shelving and drapes, and placed a used 4-drawer metal filing cabinet nearby to house equipment, books, and incidentals.
Lucien used his great design skills to make new covers for our drug and organic chemistry library. The books were now all labeled as science teaching for schools and museums. Almost no one casually looking at such a book would realize that they were really anything else.
In addition to the cover I would have used on the drive, if needed, we thought up some cover for Tom. He is developing curricula and exhibits for schools. I was there to teach him bioluminescence activities – a curriculum we had developed many years earlier called ‘Science in the Dark’. He was also learning my da Vinci programs. Tom would say, if asked, that he relocated to Portland because of his medical problems and the Death with Dignity law. He was working as a consultant and advisor in the area of science education. Although some of this cover was used in conversations with neighbors, store clerks, and visitors, no one ever came by to make a serious inquiry.
The vacuum pump and a dry ice trap were placed and installed under the table and the fume hood. Dry ice is readily available from local supermarkets and can be acquired as needed. As everything had been previously tested in Salt Lake, most of the set up went quickly.
We had previously installed a small window air conditioner to be sure the downstairs lab temperature stayed around 70 F or below.
We used a small main floor bedroom for our chemical analysis work, especially the thin layer chromatography (TLC).
“I’m a great fan of TLC,” I said. “It’s so simple, so inexpensive, so effective.”
“I remember a great set of paper chromatography activities – at OMSI,” Lucien said, referring to Oregon’s Museum of Science and Industry. “The facilitator had us write our names with black felt pen on the paper, and then separated the colors making up the black color. Cool.”
“It’s the same process as getting a celery stalk to ‘pull’ a colored dye up the stalk,” I said. “Capillarity is almost magical. Just molecules in the liquid shaking hands with those on the walls with enough strength to counteract gravity.”
“And now we’re using it to analyze illegal drugs,” Tom said, “to see if I’m still a pretty good chemist.”
“Did you see the recent story on beards and bugs?” Peter asked, stroking his chin. “Beards are loaded with bacteria and other organisms.”
“I wonder if Shulgin kept his covered while working,” I said.
“Not me,” Tom volunteered. “It’ll be largely under a respirator mask most of the time anyway.”
“And you do wash it?” I asked.
“Bonnie insists I do,” he smiled. “Time to make some stuff. Where’s that sassafras? Root beer, anyone?”
“I’d prefer tea,” said Lucien, handing Tom a bag of dried, chopped root bark with about two pounds of material.
“Two pounds, dry weight. Here’s the rough estimate: dry bark is perhaps 7% sassafras oils, via steam extraction. It’s less for the root – like only 1%. About 80 % of the oil is safrole, which we get via vacuum distillation of the sassafras oil. So a pound of dry bark – about 500 grams – gets us about 35 gr sassafras oil, meaning close to 30 gr of safrole,” said Tom.
“And I have about five pounds in this old suitcase,” I said. “It’s already in a powder form. No difference in price between bark and powder- $35/pound – from Monterey Bay Spice and Herbs.”
“The seven pounds should get us some 200 grams of safrole. If the MDMA synthesis is 100% efficient, that would mean over 200 grams of MDMA. Let’s guestimate a yield of 10% or so, providing roughly 20 grams of MDMA.”
“That’s about 200 normal doses. More than enough for our initial testing and even initial treatments,” I said.
“Time to prepare our key reagent” Tom smiled, “via steam extraction and distillation. Stand clear.”
“Talk me through all this,” Lucien said. “I want to learn some real chemistry.”
“You want to be Tom’s ‘graduate student’?” I asked.
“Why not? They don’t teach you any chemistry when you’re a Communications major – and it’s starting to seem that good organic chemistry may be the key to enhanced communication.”
“OK, but you’ll have to do some practicing and homework. Start by reading this little Organic Chem Lab Survival Manual by James Zubrick,” Tom said, pointing to his expanding chemistry library, “and watch carefully.”
“I want to learn, too,” Peter added. “I can be Lucien’s assistant.”
“I’m already a chemistry lab supervisor?” said Lucien.
“You guys start with learning the structures – the unique safrole and the magic 29 for MDMA – notice the similarity?”
Tom then set up a steam/extraction distillation unit, including condenser and needed flasks for delivery and collection. He provided a running commentary of his actions and activities. He had carefully washed and organized all the glassware and related materials needed for the various steps of the reactions. Tom’s teaching skills had obviously not deteriorated over the last 20 years!
We were on our way.
“Lots of steps for a small amount of root beer – smelling oil,” Lucien said.
“That’s why most kids don’t want to be organic chemists,” Tom smiled.
“Remember Papa Haydn?” Peter asked.
“You mean that great chocolate and pastry shop?” Lucien responded. “Yes, why?”
“I read a fascinating article in that New Scientist you left lying around – on the science of chocolate,” Peter said, looking my way.
“I remember that,” I said. “An incredibly complex process, involving many different types of fungi and bacteria.”
“If you go to Trader Joe’s, you find dozens of varieties of chocolate,” Peter continued. “Stuff with salt, with pepper, with strange flavors – and most of it really delicious.”
“And some of it very strongly flavored,” I said. “Are you thinking what you’ve now got me thinking?” I asked.
“It may be perfect to mask MDMA’s bitter taste – in a very pleasant way,” continued Peter. “After all, look what brownies have done for marijuana.”
“We can become chocoholics,” Lucien said. “I’m game.”
“You know, it can be even more useful,” I said. “It can also provide cover for us – for harmless. We’re concocting chocolate flavors – that’s why all the equipment – the lab.”
“We can be cooking chocolate while we’re doing the other reactions,” Lucien suggested. “The downside is that the chocolate aroma may well encourage walkers to stop and ask questions.”
“And we can just say we’re formulating new chocolate flavors,” Peter said. “Q.E.D.”
So I did some homework. Can we mix chocolate and MDMA? Proportions? Taste? It’s been done.
“MDMA in chocolate truffles got a UK master chef arrested back in 2011,” I reported.
“I assume he’s now in jail,” Bill said.
“Nope. He was convicted, fined, given 9 months jail time, but the sentence was apparently suspended,” I said. “I didn’t learn anything about amounts, although two kids ate some chocolate mousse laced with MDMA and got sick. The adult who ate two truffles said he had an out of body experience.”
“Has there been any follow up?” Jay asked.
“Nothing I could easily find on line.”
“Great chocolate is certainly ecstatic as well as blissful,” Bill said.
“What’s interesting is that they did detect the MDMA in the truffles and mousse, thus all the other stuff in chocolate doesn’t really mask the analysis.”
Further web searching hinted that mixing MDMA with chocolate should be fine, although absorption might be a little slower than with liquid ingestion. In searching chocolate and ecstasy all I could find is www.chocolateecstasytours.com – and not with MDMA. These are basically expensive chocolate tasting excursions. They seem to be very popular. There’s even a line of Ecstasy Elite Truffles. So perhaps that provides even more cover – we’re involved in the feelings of ecstasy delivered via chocolate.
“Remember anandamide -” I asked, “the bliss molecule.”
“As in cannabis? I remember the feel-good gene research,” said Peter.
“Exactly. It was discovered in 1992 – and four years later was found in chocolate – in very low concentrations.”
“That is really cool!” Lucien said.
“Yes – and a third or so of the US population have higher levels of the bliss molecule than the less-blissful other two thirds – and thus don’t respond as strongly to THC in marijuana – that’s the feel-good gene story.”
“This all keeps getting more and more interesting,” said Peter.
“Yes, but…” I cautioned, “the concentrations in chocolate are so low as to have very little direct effect. But that doesn’t make good chocolate any less blissful.”
“Let’s visit Trader Joe’s – and Papa Haydn’s,” Lucien suggested. “We’re all willing to put on some weight for the cause.”
There’s more to anandamide and cannabis. There’s a component in cannabis that really boosts anandamide: cannabidiol. It apparently is helpful in treating the nine percent or so of regular marijuana users who actually become addicted. And it treats the dependency by somehow boosting internal anandamide concentrations.
“So our bliss molecule is somehow tied in to marijuana?” Lucien asked.
“Yes – and not only cannabis and its components – but also to oxytocin,” I said. “Oxytocin is called the ‘bonding’ hormone and linked to social bonding and feelings of empathy. There are some studies underway to see if it might be helpful in alleviating dementia. The jury’s still out as to whether MDMA and oxytocin are connected or inter-related.”
“I saw a clip on the mdmathemovie site, where Julie Holland seemed to think MDMA did act, at least in part, via oxytocin,” Lucien noted.
“We’ll see,” I said. “The MDMA film is close to being finished and released. Perhaps the perception will change. Video segments and clips are viewable on line at www.mdmathemovie.com/videos/ .
“I love the semantics,” Lucien said. “We’re dealing with empathy, ecstasy, bliss, bonding, and also love – oxy’s been called the love hormone, you know. And now I just learned that awe is another trait we need to cultivate.”
“Awe?” I asked.
“For once I read something before you did! A NY Times op-ed: ‘awe is the ultimate collective emotion’. It binds us, motivates us to act in collaborative ways, and be more generous to strangers.”
“Sounds a bit like empathy to me,” I said. “Look out for a bunch of new studies trying to relate awe to MDMA, oxytocin, or anandamide.”
“You read those,” Lucien said. “I’d rather experience awe – and bliss.”
“I’ve been more thoroughly studying the synthetic procedures,” Tom said. The forensic papers by Noggle and friends report a seven day reaction for the bromination, followed by a four day reaction for the amination step.”
“That must be why clandestine labs tend not to use the HBr – methylamine route,” I said. “Fortunately, we’re not in a very big hurry, and we don’t need very large amounts.”
“If it’s that slow, and the yields aren’t great, perhaps the watchers will be watching elsewhere,” Peter added, optimistically.
Tom and I studied the papers covering synthesis of MDMA – as well as some clandestine lab and self-published stuff online, including the online book MDMA Synthesis for the First Time Chemist – which certainly facilitates clandestine production.
I had purchased (via Amazon!) A Laboratory History of Narcotics: Amphetamines and Derivatives. Much of the book is available on line, but it is convenient to have the information in book form. The book is very informative and complete, including a chapter on chemistry principles and one on lab techniques and procedures, a good companion to the Zubrick book. It’s apparent that the author, a Jared Ledgard, must not have had much formal education – evidenced by the spelling and semantic errors – and may be largely self-educated in chemistry, but it’s all there. The book is probably self-published and did not have any serious editing services. An Amazon search shows his more popular books are a Preparatory Manual on Explosives, and an earlier one on Chemical Warfare Agents. Interesting fellow.
After reviewing the Ledgard materials, and the other material we had read, Tom and I agreed to begin with the process described in the Noggle, 1991 papers – basically 3 key steps:
getting safrole by steam distillation from sassafras, then via vacuum distillation – which we had already done;
brominating the safrole, to get the bromo precursor of MDMA; and
swapping the bromine out with methylamine, to produce MDMA.
And finally step 4 – purification.
Tom agreed to write-up the procedures in sufficient detail, with Lucien’s help, so we (meaning Lucien) could reproduce them without Tom’s assistance, in the event we need more moksha and Tom’s no longer able to produce it. And Lucien made a fake cover for the Ledgard book, whose original cover is an ominous black with Narcotic in large font – we didn’t want any visitors or even burglars noticing it.
“We didn’t do badly; we have about 100 grams of safrole from Step 1,” Tom said, proudly. “I only used about half of our sassafras bark stock. But do get some more.”
“It’s on order,” I said.
“Given the issues with hydrobromic acid, it’s best to do Step 2 – the bromination reaction – in small batches – about 5 gr of safrole, added dropwise to about 25 ml of the hydrobromic acid.”
“You’re the chemist,” I said, putting on my safety glasses.
Lucien and Peter hovered nearby, with the requisite lab coats, nitrile gloves, and full safety glasses. Tom then poured, in the hood, very slowly, 25 ml of the acid into a beaker. He then began adding, slowly, the safrole – drop by drop – while stirring the acid solution on a magnetic stirrer. It was all done at room temperature – and to be continued for seven days!
“It’s a slow reaction,” Tom said. “I’ll start another batch every day for the next three days. Organic chemists only seem slow – the good ones are cautious and patient.”
Seven days later, Tom said, “Not bad. Looks like we got about 4 ml from the 5 ml safrole we started with. That’s an 80 % yield – by volume.”
“You are good, “ I said. “Interesting color.”
“Yes, the heavy Bromine atom changes the optical properties to a deep red and increases the density, although there could also be some free Bromine,” Tom explained. “Step 2, bromo-safrole – check.”
“Check, and the literature suggests that no additional purification is needed at this stage. Onward,” I said.
Peter and Lucien each studied the process and performed their own trial extractions and distillations. Tom would have them ‘solo’ with one of the next batches.
We cleaned up the Step 2 work and began Step 3 – which needs to react for 4 days.
The trick to chemical reaction speeds (kinetics) is to increase the rates at which the reacting molecules collide; they have to touch each other via collisions. But that’s not enough. They have to hit each other with certain orientations, so that the bonds doing the reacting can ‘hand-shake’ with each other. It may take millions or billions or more collisions before a just right one occurs. And that all takes time – entropy. Higher concentrations, higher temperatures, and higher pressures all increase the collision rates. But such super-charged conditions can also lead to unwanted side reactions, lowering yield and producing unwanted contaminants. That’s why organic chemistry is a balancing act – a delicate art – of getting conditions, and thus reactions, just right. Tom’s very good at it.
“It’s always about entropy, isn’t it?” Lucien asked, suggestively.
“You know it is,” I smiled.
“You know I still use your license plate holder – the one that says Entropy Wins!”
“Keep it,” I said. “It’s a classic.”
Four days later Tom took the Step 3 reaction container and went through the additional nine steps, resulting in pure MDMA – an oil.
“And now we have Step 3 – MDMA. Check. Now it’s time for Step 4: purification. The best description I’ve seen on purification is Shulgin’s in the PIHKAL book.”
Tom then did the eight steps needed for purification, resulting in fine, white crystals of MDMA hydrochoride salt, about two grams – more or less. Our overall yield, based on the original safrole amount, was about 40% – enough for up to 20 doses.
“Pure MDMA – real Molly,” Tom said. He carefully smelled the powder. “And no safrole smell – just a touch of ether, but that will disappear. Pure MDMA – check!”
“Time for some tester analytics – and for some analytical chemistry,” I said.
“Testers start at very low amounts and slowly work up,” Lucien volunteered, “nice and careful, like Shulgin did.”
“I‘m with you,” Peter agreed.
“We need to keep it sealed,” I said. “Exposure to Portland’s ultra-humid air is not a good way to store chemicals.”
I had brought a plastic heat-sealer for packaging the material in low density polyethylene (PE) bags. It was very fast and simple to seal 100 mg portions in small PE bags.
We discussed the private testing we would soon do. We reviewed Hofmann’s process for dealing with new chemicals as well as the more extensive Shulgin protocols. The protocol we devised for our very first batch of MDMA was;
skin tests (we expected some minor irritation due to the acidic nature of our MDMA-HCl salt),
tongue tests (ditto),
oral ingestion in orange juice (10 mg, then 50, then 100 – each a day apart).
Lucien, Peter, and Tom (for the time he’s still in Portland) would each test while being observed by the other two. We devised a testing protocol and data recording worksheet which was a bit more comprehensive and complete than what Shulgin originally used. Our data included – every hour for six hours:
sweating or flushed feelings.
The standard subjective mental feelings and observations recommended by Shulgin were used:
No effect (-) – baseline;
Very minimal (0) – perhaps placebo effect – alert;
Plus one (+), Shulgin: ‘…a real effect, and the duration but not the nature of the content can be discerned. The “alert” has progressed into something unmistakable’; clear-headed, creative, engaged;
Plus two (++) – ‘There is an unmistakable effect, and both the duration and the nature of the effect can be stated. It is at this level that the first attempts at classification can be made’; for MDMA this may manifest as openness, lack of fear, lack of anxiety;
Plus-Three (+++) – ‘…the level of maximum intensity of drug effect. The full potential of the drug has been realized. Its character can be spelled out … and the chronological patterns to be expected are defined’;
Plus-Four (++++) – ‘…the “peak experience” … a serene and magical state … the extraordinary place, that one-of-a-kind, mystical or religious experience which will never be forgotten…. in a class by itself.’ Unlikely for MDMA at the doses we are using.
We also reviewed some of the experience with low dose MDMA – the ‘creativity’ studies by Fadiman, Eisner, Beck, and others. About half of the ‘normal’ dose often resulted in enhanced alertness, creativity, problem-solving skills. Eisner claimed to write better with a little MDMA in him.
We had set up the TLC work area in a main floor bedroom, on a table just in front of a large window looking to the back yard. We had a dehumidifier in the room, to deal with Portland’s humid air. Opening the window, and using a large fan strategically placed, we were able to push the TLC solvent vapors out into the environment. Our real environmental concern is the liquid waste, which we placed in waste containers, as trained to do in university chemistry labs. We didn’t know yet how we’d dispose of that waste.
Lucien and Peter continued training under Tom, and Tom proceeded to complete the remaining batches of the synthesis over the next week. He’d observe Lucien’s and Peter’s initial, cautious personal testing.
We based the TLC work on an undergraduate honors thesis we found on line – the same one that used silver colloid – enhanced Raman for drug analysis. The student and her professor collaborated with local drug forensics labs and, through them, had access to reference amounts of MDMA. We followed their published protocol.
“Doesn’t seem to be any major contaminant,” Tom said, examining the plate.
“It looks very good,” I agreed. “Most anything else that might be there should also have separated, but with a different migration distance, resulting in multiple spots or a skewed or distorted spot.”
“So far, so good,” Tom said. “But is it MDMA?”
“And that’s where the Raman comes in. Analysis step 2 coming up,” I said.
In order to detect the chemicals present in the spot with our fiber-optic Raman unit, we needed to use surface enhancement – the so-called SERS method. Again we chose to go with the undergraduate student project process, using a silver colloid.
“Pretty good, for a first try,” I smiled.
“Damn good,” Tom said. “The spectra are essentially identical to what that undergraduate got. Our MDMA could be used as a reference!”
“Don’t get carried away,” I responded. “It looks very good – very pure.”
“This is starting to sound like that first episode of Breaking Bad,” Lucien joked. “I’m ready to test.”
“Me, too,” said Peter.
“Check,” Tom and I said at the same time.