mdp2p from oxone

[Chromic]

RWM: Oxone is a peracid, ozone will cleave the double bond... HP: I never could get the 1991 JOC ref to work with isosafrole, neither could improv_chem... psychokitty said he had success, but said his yields were low (and I'm not sure if he ever reported that he made mdma out of mdp2p)...

[noj]

potassium monopersulfate is what I used, cost US$7 for 2 lbs. Much cheaper than benzoquinone and palladium chloride. And OTC as chlorine free "shock-it". Many many thanks psychokitty and chromic!
No One's Jurisdiction

[backburner70]

(my first post!)

What type of yields are normal from the H2SO4 hydrolysis? I know Chromic mentions 50% in the writeup, is that typical? I was wondering if it was worth the effort to capture the epoxide/diol fractions and throw them back in the mix the next time around. What is the stability of these two for storage purposes?

bb 7.

[Rhodium]

Typical yields using the performic reaction is 50-60% and with the buffered performic 10-20% more than that.

[Chromic]

I saw something like 60-75% overall.

[noj]

Amalgamation worked! Not certain of yield yet but it definitely has the right taste.
No One's Jurisdiction

[Chromic]

I meant 60-75% from isosafrole -> mdp2p. Overall is something like .90 * .60 * .75 = ~40% overall molar yield of mdma.hcl from safrole.

[Rhodium]

Only that it does not require formic acid.

[noj]

Or 35% H2O2.
No One's Jurisdiction

[Vibrating_Lights]

Hello every one.  It has been a while since swim has been here.  the holidays are a busy time around our city a  we will say that this was the best new years we have ever had.  Our hats go off to Chromic again.  He is the shit. We all know that the Oxone procedure works pretty fool proof.  we have not yet done the research althought chromic might have about diffrent Ph levels.  It is their understanding that oxone will epoxidise under weakly  acidic conditions.  swim thinks that any one experiencing low yeilds with this procedure are dealing with an OTC pool store oxone source with the ingrednce listed as 85%monopersulfate compound and 15% inert.  Well those inert ingrediants are not inert for our purposes.  The so-called inert ingrediants in those 85%mixes are sodium Carbonate and sodium metaBisulfite.  Monopersulfate is an acid by itself in a saturated solution it will definatly carry a high PH.  Now the companies that mix up the oxone are doing so in a that the formula that they sell is buffered by the sodium carbonate in the same way that chromic buffers his oxone with Sodium bicarbonate. The proper ammount of 85% Monopersulfate solution to use on a 200mmole of isosafrole is around 167 grams or so that is including inert ingredients and all straight out the bag. They think peope could be getting bad results because they are adding the amount of bicarbonate that chromic suggests and the Ph goes to high lowering the solution's epoxidation capabilities. Swims recomendation is that when using 85% Monopersulfate  OTC pool formulas moniter the Ph while adding the bicarbonate and even check it before adding and aim for around a PH of 6.9  We think this might improve the yeilds for some bees experiencing this problem.Also the other ingredient Sodium sulfite will not affect the rxn.  We hope this instills cofidence in using Otc pool chems. Just check your labels.  Also Thermal Rearrangement of crude isosafrole epoxide  67% yeilds 245.c heavy stirring 2Hr reflux time with  2.5gallons of water with 500grams of ice through the recirculated through the condensor  temp was monitered at the base of the kneck and the cold water keeps most of the vapor in the flask.  moniter the progress under a black light.  As soon as you witness it under a black light you will understand. They suspect that reaction times may very depending of the ammount of side product during the epoxidation and the purity of the starting isosafrole.  They suspect that yeilds will improve greatly perhaps with the thermal rearrangement with vacume distilled epoxide. The thermal rearrangment will provide superrior yeilds because ther is no acid around to chew on the molocule which is the cause of the red coloration with the typical H2SO4 rearrangement.We believe that up to around 80% yeilds are possible with distilled epoxide. yeilds might even be higher if the Ph of hte oxone run is kept at 6.8-7 yeilding only epoxide and no glycol. they suspect that the loss in yeild might even be that glycol is not converted by either method of rearrange ment and with H2SO4 is destroyed and with thermal it it just not converted.   When they send swim their exact quantative data Swim will post.

VL_

[cheeseboy]

Tanks for da meal!
May The Source Bee With You....Always.

[Vibrating_Lights]

Chromic,  was there any indication of glocol being present when you did tlc analysis of the epoxides. we know you keep the proper PH.

[Chromic]

I didn't do TLC, I did NMR. There were two chiral centers, a mixture of R and S epoxides (I figured). I doubt any of it was glycol (when buffered with bicarbonate). Anethole epoxide rearranged very nicely to anethole ketone and the yields were excellent (both of the amination and rearrangement), and I'm sure isosafrole would do the same. I attempted it and got excellent yields of suspected mdp2p, however, I screwed up on the amination and got piss-poor yields (enough to celebrate news years eve... but not enough to post at the hive recommending this procedure to the general hive populace...)

[Stroke]

But if it was the amination that was quasi-botched and the yields of epoxide oil and finally ketone oil were good then it's fair to say that the OXONE method works well to epoxide-->ketone(MDP-2-P). No Formic OR 35%H2O2! Yum Yum

[noj]

Chromic, yields for swim turned out to be 9g of salt from 25g of ketone. This is consistent with any amalgam swim has done so it is apparently my method causing the yields. I'm not sure if it was just the 6 month absence of useage or what but that was a potent 150mg dose.

I think the commercial imports must be cutting their pills down to 40mg of MDMA because there was nothing but balls-to-the-wall reviews.
we are we are

[Vibrating_Lights]

swim would say that european pills are average 80-90mg israile middleeast 65-70.  poeple neeed to get #4caps and fill em full 126mg.
Vl_

[Chromic]

What amalgamation did you use? Your yields sound a bit low, but if it's for personal, then that's tons... Yeah, 150mg of pure mdma.hcl is fucking amazing for me too as I use only 3-4 times a year.

[noj]

The typical MM variety. The mercuric chloride was self made and the ketone may have been impure. I did notice that after checking pH while adding the sodium bicarbonate to the oxone that the amount specified made it too basic (pH so that will have to be worked out. I can't imagine why the manufacturer would buffer it since it will be added in 1 lb.(as directed) to 10,000 gallons of water.
we are we are


If one were having trouble with the solids while extracting the glycol with DCM, would toluene work if the solution was made slightly basic?

[Chromic]

Yeah, toluene would work fine. I used DCM because it's more easily recovered than toluene.

[Vibrating_Lights]

Also if you strip off your methanol by appling vacume to the  mix the solids will dissolve back in the water allowing you to skip the filteration step.
VL_