================================================================= This file is a part of the 1999 Hyperreal Drug Archives Snapshot. This snapshot is hosted by Erowid and will not be updated after October 1999. The information in these files may be out of date. See Erowid's Psychoactive Vaults for more current info. ================================================================= From: nobody@huge.cajones.com (Huge Cajones Remailer) Subject: Iodosafrole Secrets: the DMSO Method Date: 1997/05/08 Message-ID: <199705090522.WAA27743@fat.doobie.com>#1/1 Organization: mail2news@nym.alias.net Mail-To-News-Contact: postmaster@nym.alias.net Comments: Please report misuse of this automated remailing service to Newsgroups: alt.drugs.chemistry,rec.drugs.chemistry,sci.chem The iodosafrole method of producing MDMA and MDA is indeed viable; being one of those multikilagram processes here in the Netherlands someone was asking about. The key is using the DMSO method of producing anhydrous HI. NaI is dissolved in DMSO and then an equimolar amount of H2SO4 is added. Na2SO4 precips out. The reason the process works is that DMSO has the peculiar property of dissolving lots of NaI. (the solubility is much higher for NaI than for NaBr, making the HI process much better for large qty- make note of this you crank manufacturers) (will phoshorus and iodine be obsoleted?? :) And DMSO makes such acids particularly active. And HI is not likely to cleave ether substituted allyl benzenes like apiole, asarone, and methysticin. (See Feiser and Feiser in first vol. Reagents for Organic Synthesis for details) Extraction of iodosafrole left to your own imagination. Our trade secret!! Finally, amination is done at room temp with methylamine for MDMA or with hexamine (via Delepine process) to get MDA or other analog. Happy trails! Pugsley and Wednesday. ps. Wednesday says: "Wouldn't it be neat to aminate those two Kava Kava active ingredients?? HMMMM Imagine Kava at 1,000,000 potency! Will this be like the Schulgin-THC experiment? Stand by. Same Adams time, same Adams channel. From: nobody@REPLAY.COM (Anonymous) Subject: Pugsley: on Bromosafrole via DMSO Method/ Various topics, advice Date: 1997/08/31 Message-ID: <5ub2kl$qpt@basement.replay.com>#1/1 X-001: Replay may or may not approve of the content of this posting X-002: Report misuse of this automated service to X-URL: http://www.replay.com/remailer/ X-XS4ALL-Date: Sun, 31 Aug 1997 08:23:19 CEST Organization: Replay and Company UnLimited Newsgroups: alt.drugs.chemistry Congratulations to the poster on getting the DMSO method of bromosafrole synthesis to work. Its incredibly easy- but too easy for anyone to believe it works. Its the amination thats the more difficult part. Be careful if you decide to make your own methylamine via the formaldehyde/NH4Cl method- it gives off alot of methyl formate at the start, which is really nasty stuff, almost as bad as dimethyl sufate. It turns into formic acid in your lungs. Big Mr. Yukk sticker on that one. Another chemical given off, formylal, has a nice smell and is relatively safe, but masks the danger involved. I'm still interested in hearing in this NG from anyone doing the Delepine reaction with hexamine camping fuel to get MDA. Bromosafrole has given mixed results. Iodosafrole works at room temp. I don't see too much problem with getting NaI, since it can be diverted from table salt and photographic applications. I don't know if CRSB sells it, but they should. (if they stay in business) I don't think that meth labs use it, since in aquious media, H2SO4 turns it into elemental Iodine plus whatever salt of Na. DMSO doesn't suffer from that problem. I still see a lot of synthesis and talk on methcathinone. Very little said about cyclization products, which is one of a couple reasons some people can't seem to make it. There were some posts here a while ago referencing the specific papers on the subject. I didn't have to time to go to the library and dig all that stuff up. Never keep academic papers or chemistry books of any kind on your property if you are making "stuff". Memorize, memorize, memorize. Try to use anything but commercial glassware if you can. A suprising amount of chemistry can be done with spagetti sauce jars and various types of tubing. Even holes can be drilled in spagetti sauce lids and brass pipe fittings soldered, for various operations involving gases. For exampe, I performed the entire asarone and anethole pseudonitrosite syntheses for TMA and PMA respectively, using nothing other than sauce jars and a large pyrex juice dispensers as containers. One sauce jar has two fittings attached to it so that an outlet tube for the N2O3 could be attached, plus an inlet for air from a fish tank bubbler. The pyrex juice dispenser was used to contain the etherial solution of essential oil. (By the way, PMA or 4-MA as Schulgin calls it, is quite the roller-coaster ride. Except you start out at the top of a gigantic hill, instead of gradually making your way to the top. And it hits real suddenly.) I think a DA would really think twice about going after someone who had no paper evidence of drug chemistry efforts, and just a bunch of old jars lying around. If you ever read accounts of DEA busts, they always tell about all the drug and bomb making Loompanics books they find. If all they find are Nancy Drew mystery novels, they'd look pretty silly. Various people have been asking about where they can buy essential oils. There are a number of web site based mail order suppliers. Just type "essential oil" into AltaVista. For example 16oz of anise oil costs $12. Same price for sassafrass. Calamus oil costs anywhere from $60-200 for 16oz depending on where you buy it. Make certian to get the Indian oil. The others have no asarone in them. Nutmeg and elemi oil are reasonable also. Parsley seed oil has gone up to about $100/16oz. If you isomerize it to isoapiole, it makes way cool DMMDA. Well, thats all the comment I can think of for now. I really haven't been doing much in quite number of months. I get burnt out on making drugs and find new interests. I've never had any desire to make money that way. After all, anyone smart enough to make their own druggs can probably make alot of money legit. Its always been a curiosity thing. I am eagerly awaiting Fester's "Advanced Meth Chemistry Book". That should be interesting. Wednesday sends her good wishes. Best Regards, Pugsley From: jrhardin@mail1.sas.upenn.edu (Josh R Hardin) Subject: Pugsley & Wednesday Please Read Date: 1997/09/07 Message-ID: <5uv3gt$mu$1@netnews.upenn.edu>#1/1 Organization: University of Pennsylvania Newsgroups: alt.drugs.chemistry,rec.drugs.chemistry First, let me thank you for the excellent information about the DMSO-Bromosafrole method. For those of you unfamiliar with it, I strongly suggest searching dejanews. Basically, it uses DMSO, NaBr (from darkroom supply houses), and H2SO4 (drain cleaner) to synthesize anhydrous HBr which converts Sassafras oil to Bromosafrole. This method is better than using commercially available HBr. The authors suggest that after obtaining Bromosafrole, a 5g tablet of Hexamine camping fuel can be added to start the Delepine reaction to convert it to MDA. Does anyone have any references for the Delepine reaction? Is the mixture refluxed, cooked in a pipe bomb, or allowed to sit for a period of time? Does anyone have any numbers? The other method of converting bromosafrole to MDA via ammonia and isopropyl alcohol or ammonia hydroxide gives poor yields (20%) and doesn't smell too good to the neighbors. In another post, Pugsley discusses iodosafrole. This method uses DMSO, NaI, and H2SO4 to yield anhydrous HI. NaI is easily diverted from salt licks. I believe that the recipe is 100ml chilled DMSO + 7.8ml H2SO4 + 43g NaI. Although this can be used for making speed without having to purchase red phos or iodine, can it be used for MDA? If one were to use the HI to convert sassafras oil to Iodosafrole, could it be converted to MDA via the Delepine reaction? How? Let's use the example of 5ml Sassafras oil + 100ml DMSO + 7.8ml H2SO4 + 43g NaI. After it has reacted for a day or so, there should be iodosafrole - right? Now, would adding a 5g Hexamine camping fuel tablet start the delepine reaction? What are the times and methods - reflux, bomb, let sit? How do the yields compare to the bromosafrole methods? Finally, in their amazing post about pseudonitrosites, the authors state that the method can be used on various propenyl benzenes. This would allow isosafrole to be easily converted to MDA. Howver, in Fester's Practical LSD Manufacture, he states that it will work on all propenyl benzenes EXCEPT isosafrole. Howver, the two procedures are different. Will it work? What is DMMDA like? Thanks for the help. BTW, please do not respond to this e-mail account. It is not mine. I can be reached at: iodosafrole@hotmail.com Thanks, HI Guy From: Secret Squirrel Subject: COME MOCK MY DMSO FAILURE (for kkplli) Date: 1997/06/03 Message-ID: <19970603141716.9331.qmail@squirrel.owl.de>#1/2 Comments: Please report problems with this automated remailing service to . The message sender's identity is unknown, unlogged, and not replyable. X-XS4ALL-Date: Tue, 03 Jun 1997 16:48:36 CEST X-To: mail2news@basement.replay.com X-Mail2News-Info-Url: http://www.replay.com/mail2news/ X-Mail2News-Errors-To: postmaster@replay.com Organization: mail2news@replay.com Newsgroups: alt.drugs.chemistry,rec.drugs.chemistry OK, kkplli, you got it. I can't stand Gwen, BTW. Let me first apologize for the outburst. After investing so much time and energy into the project, to have it fail miserably at the end was frustrating, to say the least. I greatly appreciate Pugsley's and Wednesday's contributions to poor chem trench grunts everywhere. That said, prepare the mudslings for my crappy technique. Keep in mind none of this actually happened and the entire post is pure fiction :). The DMSO was purchased anhydrous at the local homeopathy shack (it even says "for use as solvent only" *grin*). It would freeze solid when put in the fridge (a good sign). Kodak anh. KBr (from darkroom supply) was used in place of NaBr, molar scaled up of course. Sassafrass oil was used straight to take advantage of eugenol, etc. I was unable to locate ocotea cymbarum locally. The relative quality of the essential oil I have no idea nor reference for, all that can be said is that it was expensive. 175ml DMSO was chilled(frozen) in an acetone-rinsed 500ml round-bottom and the flask placed in an ice-water bath. There was then added 30.6g H2S04 drain cleaner with some evolution of heat. The drain cleaner was slightly discolored brown even though it came from a sealed container (although the container is probably a year old). Looking at the container now, the acid is dark brown-red with chunks, disgusting; evidently I had drawn off the undisturbed clearer top part when doing this, but still undoubtedly introduced impurities. I hadn't realized it at the time, or even much later. 69.3g KBr was then added. The initial granules falling into the flask produced a fine mist, much like ammonium chloride forming above a bottle of muriatic and a bottle of ammonia placed next to each other, which shot up a bit and gave me a bit of a gag. Perhaps the addition order should be reversed. The soln turned orange, and began to stink. The stench is a lot like garlic, and exactly like the smell of the sweaty guy who had the locker next to mine in high-school gym class (ugh). A lot of KBr remained undissolved despite repeated stirring with a glass rod, as expected. 10ml sassafras oil was pipetted in. The stink changed from garlic/sweat to garlic/sweat/bandaids. The soln turned brownish-red with a sort of mobile greenish band on top. The flask was tightly stoppered, then entirely enclosed in a ziplock bag, which still didn't keep in all the smell, and left on a dark shelf at room temp for 2 days with occasional swishing and/or stirring. It turned entirely brownish-red. The solids remained on the bottom throughout, being broken up upon stirring. My notes are missing for the next part, but around 600 ml of distilled water was added in two portions, the entire thing getting dumped into a liquor bottle. A dark red, clear oil settled to the bottom; the aqeuous layer turned cloudy tan as the solids dissolved into it. The aq layer was poured off, and the oil washed with a bit more H2O. Yield of oil was (guessing) maybe 7 or 8 ml. To the oil was added 400ml denatured alcohol and 10.2g crushed camping fuel, which was used straight but was nice and white crystalline. A few small pieces of fuel didn't dissolve right away, but had after the soln sat one day. The soln was left alone until the 3rd day, when heating was attempted, but aborted due to pesky interlopers. The 4th day the soln was finally refluxed on steam bath for about 6 hrs. It sat one more day (good undisturbed lab space is hard to come by). The soln remained a reddish tea color. 50ml muriatic driveway cleaner (31.45% HCl) was then added in increments. The first 20ml produced loads of fine white needle crystals, filling the 500ml flask halfway and nearly giving me a heart attack for the few seconds until my brain realized there were just too many and they were probably ammonium chloride and unreacted hexamine. As the rest of the HCl was added, the crystals all dissolved, but then gradually a white ppt formed, snowy and unlike the needles. The flask was refluxed on steam bath about 4 hrs and then sat for a day. The ppt did not dissolve with heat. 125ml H2O was added, which dissolved the ppt and turned the soln opaque tan. A dark clear red oil settled out (I assumed it to be unreacted bromosaf). The pH at this point was less than 3, determined by indicator paper. The oil was seperated and the aq soln extracted with 3x20ml 1,1,1-TCE. The TCE extracts were combined w/ the oil and set aside. 80ml 25% NaOH (lye) in water was added to make the aq soln strongly basic. After shaking, a (small amount of) red-brown oil settles to the bottom. The oil was sep'd and the aq layer extracted with 3x20ml 1,1,1-TCE. The TCE extracts were orange-ish. The remaining aq soln looks like iced tea. Post-mortem dissection of my notes reveals the combined TCE extracts and oil did not get an additional water wash. The TCE was distilled off in a flask I finally remembered to tare beforehand, leaving 7.4g of a dark black-red oily goo, which was dissolved in 12.5ml anh. isopropanol and treated with a couple ml of HCl, then evaporated on steam (ala ZWITTERION, remember him?) to give a disgusting orange tar (which had to be scraped off with acetone), a few grains of probably NaCl, and a whole lotta stink. I would guess the stink was from methylamine HCl (from unreacted hexamine hydrolyzed during the second part of the Delepine) subliming with the heat; it smelled kind of like burning plastic. A cold beer was then searched for, to no avail, at which point a mentally and physically exhausted fetal position was assumed, with soft crying. For my next attempt, I'm considering (among other things) doing the first part of the Delepine in TCE instead of alcohol, which would allow me to see the progress of the rxn, harvesting the pptd hexamine salt and returning the rest to the heat. The salt could then be hydrolyzed in a separate reaction. I'm also considering use of the bomb. Constructive flames appreciated. From: "glowbal" Subject: Re: Repost: Fester on Bromosafrole Date: Sat, 22 Nov 1997 00:00:00 GMT Message-ID: <657ek3$9bq$1@newshost.cyberramp.net> References: <3474A629.5BC6@Z.Z> X-MimeOle: Produced By Microsoft MimeOLE Engine V4.71.1008.3 Organization: posted via: CyberRamp.net, Dallas, TX (214) 343-3333/(817) 461-8484 for info Newsgroups: alt.drugs.chemistry,rec.drugs.chemistry >PREPARATION OF BROMOSAFROLE >FROM 48% HYDROBROMIC ACID > > > >A greatly improved procedure using 48% HBr to make bromosafrole is my >own invention, and it is with >unbounded pride that I offer this advance to the field of MDA >manufacture. This procedure is both >quicker and much higher yielding than the procedure worked out by the >jackass who wrote the article for >the Alabama Academy of Science If I may repost an intesting artical yet once more for further discussion related to bromosafrole. (Here is the only bromosafrole (or bromo propenylbenzene) synthesis you will ever need. It proceeds totally anhydrous with pure reagents, and generates no obnoxious fumes to give you away. More than likely, this will spur DEA to add new watched chemicals (like what isn't watched already- air, water, ?) To 100 ml of chilled DMSO add 7.8ml conc. H2SO4 (i.e. drain cleaner). To this add 30g of NaBr. Stir well and repeatedly. Solution will turn orange as all the NaBr is turned into Na2SO4. Do not filter, leave crystals alone in case there is some unreacted NaBr left. If the H2SO4 and DMSO is anhydrous, so will the HBr be anhydrous. Add 5 ml of sassafrass oil. Or scale qty of everything up for more sassafrass. Let sit at room temp. Don't bother to filter out crystals, in case there is unreacted NaBr. In 1 or 2 days solution will proceed as in Fester's turning green, then purple, then gradually burgundy. To understand why this works so well, see Fieser and Fieser "Reagents in Organic Synthesis" under DMSO monograph. Note that there are two pathways for HBr to react. Via an ionic mechanism gene rates the desirable compound. Via a free-radical route forms terminal bromo compound, which cannot be used (you can try for interesting analogue, but who cares now that all mind altering chemicals are illegal under the Analoges Act, including all those in everyone's brains- imagine, even Jesse Helmes committing felony if he has any brain cells left). The crude sassafrass oil contains eugenol, a phenolic compound which inhibits free radical reaction. Thus you will get better product if you don't purify out safrole. Also keep reaction mixture away from air and UV light, both generate free radicals. The final mixture gets 500-1000ml of water added. The crude bromosafrole which settles to the bottom is seperated without adding any organic solvent. If you cool it it gets pretty sticky and syrupy so the water layer can be just poured off.) It has been reported that many notice a very mild color change in this synth over the recommended one to two days. The DMSO appears to allow the addition of large amounts of acid without degredation of product, leaving the reaction mixture a light yellow and the bromosafrole orange. Does anyone have any ideas why the mixture does not proceed in the traditional color chages that Fester often indicates. jeffamine hcl From: "guest" Subject: Re: Re: MDA from MDP2P Date: Sat, 08 Nov 1997 00:00:00 GMT Message-ID: <01bcec6e$4d0ee230$0701000a@wkst7> Organization: Wisper Newsgroups: alt.drugs.chemistry On Fri, 07 Nov 1997 03:12:49 -0500, notyet wrote: > Man, this has to be some of the most confusing research I've done. > Could someone (Eleusis, maybe....) tell me exactly which method for > brominating safrol with 48% HBr actually works. My #1 so far seems to > be starting with MDP-2-Pol and brominating like Fester told us way back > when chemistry worked differently (apparently). This would seem to > drive the reaction towards the bromnation side, due to the willingness > of that alcohol to leave in place of Br. > So c'mon, gimme some insights. Why don't you try doing a bit a basic research? Visit a library. In the library you will find books that you can read. When you've discovered how it's done you can post your results to a.d.c for the rest of us to read. You can connect to www.deganews.com and read old Eleusis and ZWITTERION posts on this topic. I include a couple below. Otherwise you'll have to contend with me taking the piss out of you. And when you've made your halo-safrole what next? The yield of MDMA from halo-safrole is shit because the main reaction is the elimination of HX to give you the alkene (safrole) back again! If I had MDP-2-Pol then I wouldn't want to brominate it at all. I'd oxidise it to MDP-2-P and reductively aminate the ketone to MDMA. If I wanted bromo-safrole I'd make it from safrole using a phase-transfer catalyst to allow non-polar safrole to mix with polar aq. 47% HBr. More likely, I'd use aq. 37% HCl or, I presume, even aq. 32% HCl would work to give chloro-safrole. See: Addition of hydrohalogen acid to alkenes: Landini & Rolla, JOC 45, 3527, (1980). JOC = Yes, that's Journal of Organic Chemistry to you. Phase-transfer catalysts can be extracted from hair and fabric conditioners. The cationic surfactants mentioned on the ingredients of such stuff will easily suffice as phase-transfer catalysts. But remember, when you use a surfactant to mix two immiscible phases you must stir them at 500 rpm or better, otherwise nothing will happen. Keep the temperature on the low side otherwise you'll zap that delicate methylenedioxy bond. So, why are you phaffing about with 47% HBr when you can walk over to the local hardware shop and do something similar with 32% HCl? Eleusis contends that aq. 47% HBr can't be used to make bromo-safrole under normal conditions. This is the original article that sparked it all off, where Carter describes the addition of HBr to Alkene. H. E. Carter, Metabolism of Amino Acids, J. Biol. Chem. 108, 1935, p 623. 200 gm. of glacial acetic acid containing 150 gm. of hydrogen bromide were placed in a 500 cc. bottle in an ice bath and 100 gm. of allyl benzene were added. A rubber stopper was wired in the bottle and it was allowed to come to room temperature slowly with occasional shaking. In 10 to 12 hours the original two layers merged into a clear red solution. After 24 hours the contents of the bottle were poured on crushed ice. The crude bromide was separated and the water layer extracted with petroleum ether. The two fractions were combined, washed with water and sodium carbonate, and dried over anhydrous sodium sulfate. The petroleum ether was distilled through a 20 cm. column and the residue was fractionated. The yield of crude bromide (90-95 per cent pure) was 235 gm. (92 per cent of the theoretical amount). Fester's method is, I believe, on the hyperreal server. Eleusis contends that Fester was talking through his arse when he described the prep. of bromo-safrole using this method. By implication, Eleusis implies that most of the rest of Fester's book is made up. > Subject: Re: Please repost: Uncle Fester review [reposted - long] > From: eleusis@netcom.com (Eleusis) > Date: 1996/03/19 > > A Thorough Thrashing of Uncle Fester's "Secrets of Methamphetamine Manufacture" > > [snip] > > Chapter 14 > ---------- > > [snip] > > The chapter gets even better, though, as Fester illustrates his greatest folly > and the one most damaging to his credibility in my eyes. > > He runs off on a tangent about making MDMA, which seems interesting enough, > but what works for allylbenzene does not necessarily work for safrole (though the > converse is true). Safrole cannot be brominated by 48% HBr. Period. In order to > have a fighting chance at bromination, sulfuric acid *must* be added, or 66% HBr, > as stated in Chemical Abstracts 14350, 1961, must be used. > This isn't just a problem of having enough moles of Br available, as Fester foolishly > assumes, but is also about having enough *concentration* as well as a suitably > solving matrix. If you can't get safrole to dissolve enough so that contact with > Bromine ions is made, how can it brominate? It can't! > > A phase transfer catalyst which can transport Br ions would be an acceptable > modification, perhaps, but as it stands, this will not and does not work. > > No, heating it won't change it, either. > > Let's assume that you do get 66% HBr made and are successful at brominating > safrole at the number 2 carbon on the aliphatic chain. Great, does this mean that > the "bomb" will still work? Yep, but what a shitty way to replace a halogen with an > amine function. > > See future posts by moi on alternative methods of doing this. It is beyond the > scope of this book review at this time. > > FWIW, though, the total yield of the bromination/bomb process is *comparable* to > the total yield of Dr. Shulgin's methods, even with all of the improvements > ZWITTERION and I have posted. > > Something to think about, anyhow. > > Subject: Re: HBr + Safrole = ?????? > From: eleusis@netcom.com (Eleusis) > Date: 1995/10/15 > > In article <45nth1$ack@newsbf02.news.aol.com>, truublonde@aol.com (TruuBlonde) wrote: > > So Fester is a Puss Face? Is the HBr route to MDA a total waist of time? > > The reaction appears feasable on paper. Does it work at all? Or are the > > yeilds just pathetic? What modifications would one need to make to this > > reaction in order to successfully synth. MDA? Any good HBr synth > > directions??? Any good alternatives? And guys, please DO NOT Email me - > > HA! > > Reload old articles, starting about 2 months ago. This has been thoroughly hashed > over. In fact, I just posted a synopsis answer to this question about a week ago. > Surely that article is still on most servers. > > Anyway, if I *were* to do it, I would consult the original H.E. Carter article, where > I would find the following corrections to Fester's questionable chemistry deviations: > > 1) anhydrous HBr gas is dissolved in glacial acetic acid, not Hydrobromic Acid, > and definitely not the azeotropic acid. > > 2) 100g of allylbenzene was used in Carter's, 100g of safrole is specified by Fester, > but allylbenzene has a mol. weight of 118, while safrole is 162. That means that > Carter was brominating .85 moles, while Fester is attempting to brominate 62. > Fester didn't even bother converting molar quantities! > > Etc... Otherwise, the process seems facile. > > Subject: Re: MDA from MDP2P > From: eleusis@netcom.com (Eleusis) > Date: 1995/11/01 > > For example.... > Bromination of Safrole at the secondary carbon of the double bond proceeds > at less than 5% yield if 48% HBr is substituted for 66% under pressure, at which > point yields are closer to 85% (J.Bio.Sci. v108). > > ..This is a "minor detail" that changes yield by 80 percentage points. > > From: nobody@zifi.genetics.utah.edu (Anonymous) Subject: Pugsley's bromosafrole prep Date: Fri, 28 Jun 1996 00:00:00 GMT Message-ID: <19960628093332.aaaa004zP@babyblue.cs.yale.edu> sender: daemon@cs.yale.edu organization: Yale CS Mail/News Gateway newsgroups: alt.drugs.chemistry Here is the only bromosafrole (or bromo propenylbenzene) synthesis you will ever need. It proceeds totally anhydrous with pure reagents, and generates no obnoxious fumes to give you away. More than likely, this will spur DEA to add new watched chemicals (like what isn't watched already- air, water, ?) To 100 ml of chilled DMSO add 7.8ml conc. H2SO4 (i.e. drain cleaner). To this add 30g of NaBr. Stir well and repeatedly. Solution will turn orange as all the NaBr is turned into Na2SO4. Do not filter, leave crystals alone in case there is some unreacte d NaBr left. If the H2SO4 and DMSO is anhydrous, so will the HBr be anhydrous. Add 5 ml of sassafrass oil. Or scale qty of everything up for more sassafrass. Let sit at room temp. Don't bother to filter out crystals, in case there is unreacted NaBr. In 1 or 2 days solution will proceed as in Fester's turning green, then purple, then gradually burgundy. To understand why this works so well, see Fieser and Fieser "Reagents in Organic Synthesis" under DMSO monograph. Note that there are two pathways for HBr to react. Via an ionic mechanism generates the desirable compound. Via a free-radical route forms terminal bromo compound, which cannot be used (you can try for interesting analogue, but who cares now that all mi nd altering chemicals are illegal under the Analoges Act, including all those in everyone's brains- imagine, even Jesse Helmes committing felony if he has any brain cells left). The crude sassafrass oil contains eugenol, a phenolic compound which inhibits free radical reaction. Thus you will get better pr oduct if you don't purify out safrole. Also keep reaction mixture away from air and UV light, both generate free radicals. The final mixture gets 500-1000ml of water added. The crude bromosafrole which settles to the bottom is seperated without adding any organic solvent. If you cool it it gets pretty sticky and syrupy so the water layer can be just poured off. Then you add 200ml of ethanol and a 5g tablet of hexamine camping fuel to start the Delepine reaction- you get MDA as the end product. (Well, if you like MDMA better you can do the tedious methylamin synth in Festers book or Org. Synth. Look out for met hyl formate which is deadly insidious poison like dimethyl sulfate) For the Delepine reaction you can use the bomb or reflux overnight, which definitely works. some experimentation is needed here since I still am unclear as to how much time this takes, or if it really can be run at room temp. The reaction with the iodo intermediate can certainly be run at room temp, but that requires a conversion to the iodopropenylbenzene comp with NaI and maybe phase transfer catalysis or insitu with NaI during the bomb or reflux. When the hexamine salt is prepared in solution, then some HCl is added and again refluxed overnite. again, possibly this can be run at room temp over several days- who knows? Then use typical amine seperation to get the pure product from the acidic mixture. Love and trips, Wednesday.