MDMA Sulfate

[Vibrating_Lights]

Does sulfate salt of MDA/MDMA have the same effect as the HCL salt? would product weight remain the same?

[PrimoPyro]

Yes it has the same effect, and NO the weight will differ. The molecular weight is different, use a periodic table and a calculator and some basic high school math to convert.
Of COURSE we don't know what we're doing! That's why it's called research!  (boom...)    

[sunlight]

The problem with the sulfate salt is that it can contain small amounts of sulfuric acid that will degrade the product (while HCl is a gas and disappear). Anyway you can expect that it will be fine months if washed with acetone (I can say it works with amp and 2CH sulfate), and years if you remove the acid with recrystallization.

[Rhodium]

Another problem with sulfate formation is that you can get the acid salt MDMA*HSO4 (with a free acidic proton) instead of (MDMA)2*SO4 which is a neutral salt. You must not overshoot the equimolar amounts of sulfuric acid to amine here, so weigh both the distilled freebase and the sulfuric acid very exact, and always recrystallize from IPA/ether or perhaps IPA/pet ether afterwards if you are going to make the sulfate salt.

[CANetics]

What is the best way to create MDMA sulfate from base?  Would it be okay to follow the same general procedure, as in the following posts? for MDMA?

Post 101320 (missing)

(psychokitty: "Re: How would correctly crystallize w. H2SO4 ?", Chemistry Discourse)

Post 101323 (missing)

(Night Trojan: "Re: How would correctly crystallize w. H2SO4 ?", Chemistry Discourse)

Post 183054 (missing)

(sunlight: "Re: How would correctly crystallize w. H2SO4 ?", Chemistry Discourse)

SWIM's plan is to titrate H2SO4/IPA into dry freebase/toluene solution to Acidic.  Filter and repeat. until no more crystal come off. Recrystallize.  Will this work ok for MDMA?

Are there any other solvent pairs that would work well to recrystallize MDMA sulfate? (SWIM has no ether)

During salt formation would PH be a good enough indicator of an endpoint?  If so what is the exact endpoint to avoid MDMA*HSO4 formation?  (precise molar measurements are not an option here as SWIMs scale is not exactly on the money...but SWIM can titrate with a nice PH meter)

What else is so bad about the sulfate salt? It seems like these impurities can be removed with a careful recrystallization or two...Why do more bees not opt for this method of salt formation?

[hest]

When I'm making amph. sulphate i disolve the freebase in methanol (app. 1g to 20mL MeOH) then drip sulfuric acid disolved in methanol (30%) into the methanol solution. When the methanol solution is acid (weth pH paper) it's all done.
I seem to remember that the sulphate salt off meth. is quite hygroscopic, but i have no idear abouth the MDMA salt

[Rhodium]

Hest: Most amphetamine salts are very hygroscopic, the sulfate and the phosphate being the less hygroscopic ones.

What is your typical sulfate yield from the freebase using that method?

[hest]

Almost kvantitative (>95%) I loos some with that amounth of solvent but who cares.

With hygroscopic i ment that it litereal melt (hydrates) within houers.

[Rhodium]

There aren't very many here who have made "regular" amphetamine, almost only meth. I would be interested in what method you used, and perhaps even a writeup, I have almost none on my page compared with the tons of meth stuff.

[hest]

I'm not a big fann of meth (stayes too long in the system)
I'll make a writeup if you want but i usual don't use a otc method. Condense benzaldehyde with nitroethane and then reduce the nitropropene with LAH

[Rhodium]

Yes, please do a detailed writeup on that method with yields and all. What I am especially interested in is the method for and isolation of the intermediate nitroalkene, as many people report difficulties with the crystallization.

And as an important note - I am not a big fan of OTC methods for the collection on my page, I am looking for as many routes as possible (preferably optimized) to all possible psychoactive compounds.

If you have other things you have been playing around with that is not yet on my page, please make writeups of them for me.

[sunlight]

I made amp sulfate years ago with a regular Leuckart with homemade am formate and P2P, not impressive yields, 30-40 %. Nothing new.

[terbium]

Interesting, about the same yields as I have found when using the Leuckart to produce methamphetamine. Some people here had claimed that when the Leuckart was used for plain amphetamine it gave better than the 30-40% yields I found for methamphetamine but I remain skeptical.

[Osmium]

Same outcome for me.

[Rhodium]

Nice. Give me a detailed Leuckart procedure for the synthesis of amphetamine then