swank (Stranger)
12-25-02 05:01
No 392627
      Anyone found a demethylation method for eugenol?  Bookmark   

Has anyone found a proven, decent yielding method for demethylating eugenol into allypyrocatechol. Swim has been doing alot of reading but all he/she has found have been unproven methods. Should swim (who is not a chemist) abandon the thought of using eugenol as a pre-precursor en-route to MDA? Is there a better starting point to focus on? Any help would be greatly appreciated. Merry Christmas everyone!
(Hive Addict)
12-25-02 07:04
No 392638
      eugenol  Bookmark   

there are a couple of PROVEN methods on Rhodium's site.  However, they are not optimized and lack OTC'ness.  however, the procedures are easy and quick.  if you have the materials, the synths are easy enough. 
(Result of Norwegian Drug Policy)
12-25-02 15:08
No 392693
      Lead the way!  Bookmark   

There are plenty of almost-OTC methods to de-methylate
eugenol, why don't you try them out, seeing as eugenol is
dirt-cheap.. smile

Somebody has to do them first, and it might as well bee you!

Bee where
(Hive Bee)
12-25-02 17:12
No 392714
      Suggestion  Bookmark   

I suggest you to first take a GOOD LOOK at Post 381882 (GC_MS: "Eugenol -> elemicin and myristicin", Novel Discourse) if you have any plans in using eugenol for anything. GC_MS did an excellent work in that area.

"Turn on, Tune in and Drop Out"
12-25-02 20:55
No 392779
      Thanx!!!  Bookmark   

Many thanks y'all!! I really appreciate the help. BTW, swim is currently looking into OTC possibilites in vet medicines. DMSO can be found at ANY vet clinic as well as dexamethazone, phenylbutezone, and a butt load of various anti-histamines. Everybody probably already knows this, but swim will keep you posted on what he/she finds anyway.wink
(Hive Bee)
12-30-02 12:47
No 394138
      demethylating  Bookmark   

SWIM recently has also decided to give up the sass digging.  Mainly cuase it's a pain in the ass.  The future lies within eugenol, it's easy and cheap to get.  The route SWIM is looking up to is pretty much all OTC, except the tetra-n-butyl ammonium iodide, which is a commonly available PTC (otc enough for SWIM).  Looked up essential oil dealers and was able to purchase a few kilograms of clove oil (~95% eugenol) for a good price, no problem.
SWIM is just waiting on a helium tank right now (for inertness), but funds will soon permit (sucks, spent like 5 g's on glassware, and SWIM is to broke right now to buy chems, even with his/her big ass jars of eugenol sitting around).

The good stuff:
Anyways, SWIM is gonna setup a two kneck rb flask with reflux condensor (liebig of course), and the other kneck with a pressure equalized addition funnel.   At the top of the funnel, a one hole stopper is put in place.  A rubber hose goes from that into a gas trap.  Another one hole stopper would be placed in the condensor.  A rubber tube would run from that hole to a regulator and a helium tank (looking into buying N2 tanks to, see SWIM has paintball guns, so stuff like this is no problem).  The equipment would be charged with xylene and aluminum foil, and flushed with helium.  Also, the addition funnel is charged with eugenol before flushing.  The xylene will be heated to reflux, and iodine slowly added down the condensor.  The iodine will be added slowly over time.  Once all the aluminum has been reacted to form AlI3,  heat would be removed, and a constant positive pressure will be kept with helium to prevent suck-back from the trap during cooling.  Once cooled to room temp, a PTC is added (tetra-n-butyl ammonium iodide) to the eugenol in the addition funnel, along with some extra xylene to dissolve it all (actually SWIM'll do all this before even putting it in the funnel).  The is added to the xylene/AlI3 mixture.  Refluxing is commensed after addtion to complete the reaction.  When finished, workup will inculde hydrolizing the mixture with H2O, suction filtering out the precipitate.  Then adding that to some ethyl acetate, and suction filtering that mixture.  Any water collected by the ethyl acetate is separated, and the ethyl acetate evaporated to yeild 3,4-dihydroxyallylbenzene.

Next SWIM was gonna use the same setup of glassware for methylenation.  This time, the still flask is charged with DMSO and good ol DCM, and this is heated to refluxing.  A solid mixture of 3,4-dihydroxyallylbenzene and NaOHis added slowly, with stirring.  After everything is added, SWIM will reflux for a while, then add a little more DCM and NaOH, and continue.  When done, shit will be setup for normal distillation.  Water is added to the reaction matrix, and also to the addition funnel.  The safrole is steam distilled out of the mixture.

SWIM was then gonna proceed with a wacker, fraction vacuum distillation with column, then nitromethan/AlHg to MDMA.
ANy thoughts?  The demethylation/methylenation comes pretty much straight from Rhodiums.  SWIM actually is looking into helium tanks tomorrow.  So results will be posted soon!