11-20-02 15:54
No 381693
The following post contains what should be close to a work-able synthesis of MDMA that is to be carried out on a very small scale. Each of the three primary reactions are to take place in a single 250 mL 3-neck flask! There is nothing at all new about what is being proposed as the Benzoquinone Wacker oxidation and Al/Hg reductive amination are probably the most reliable procedures used today for this purpose. However, there are a few reasons why I think it would be helpful to discuss the dynamics of these reactions at such a small scale. One is that many bees do not require much honey, so something like this might suit their needs perfectly. The other is so a good method exists for a new bee to practice with that is fairly simple, would allow for several mistakes without wasting much chemical, and the chance of success is still a high one. In fact, less than 3 ounces of sassafras oil, 50 grams of Benzoquinone, and a gram of Palladium Chloride will be enough for nine trials at this scale! You see, after the distillation has completed and 60 grams of safrole have been isolated, there is enough product to attempt the Wacker oxidation three times (since only 20 grams of safrole are needed). A successful run should result in around 15 grams of MD-P2P, of which only 5 grams are used in a single trial for the subsequent reductive amination step. So even if your lab skills suck (like mine do, even though they shouldn’t!), you still might get this one right on the ninth try, so could consider the effort an unqualified success!
I thought it would be better to give a brief explanation (or maybe justification) as to why this synthesis might be important as opposed to just posting it. One reason is because I’m worried about being trashed for writing such a long document that is just a re-hash of someone else’s work and how all my problems would be solved if only I UTFSE more often. But I also think it is possible that some experienced bees would appreciate something like this and might even want to give it a shot. After all, the whole synthesis can be completed within a 24 hour period! So why not, since some of you must have really big plans for the weekend? And we all know about how old stuff that’s been sitting around for who knows how long can’t even come close to a batch of honey that is so fresh and so clean as this one will bee!!!
(Hive Bee)
11-20-02 18:42
No 381748
At least buy a one liter. Your not going to be able to pull it off the whole way through with a 250, if only for the fact that you need overhead in the Al/Hg.
If you are serious about this here are your minimum requirements.
1 hotplate/stirrer combo
500 mL flask/ 250 ml flask
2 L erelynmeyer flask
200 mm condenser
HPVAC vacuum pump
Be prepared to spend several hundred dollars.
Pr(+)tium
(Hive Addict)
11-20-02 19:01
No 381754
Yeah, and if your gonna go small, make damn sure to get small sized glassware, you dont want to try distilling 20 mls of freebase in a 250ml flask, youll loose too much to mechanical loss. But I really dont see the utility of it, as each time you assemble all the components, your taking a risk. Better a couple of larger reactions than several smaller ones- pretty much the same amount of time and effort barring slightly longer distillation times. Make friends with Mr. Shovel if your worried about holding on to quantity. If its just personal use (and you know damned well things never turn out as first expected
) a couple of rxns should last you good and plenty.Im not the bearded man upstairs, Im a bald guy with a healthy penis. So open yer pie-hole!