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Gassing with mineral spirits

Started by wolfx, April 11, 2001, 10:13:00 PM

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wolfx

Is it OK to use mineral spirits with an HCl gas generator
for MDMA ? Do I have to distill it first ? What would be
the best solvent for this ?

terbium

You can't get toluene? It is probably a better solvent for the freebase. But if you can extract your freebase into the mineral spirits then it shouldn't be any worse for gassing than toluene.

I think gassing in toluene (or mineral spirits, or Colemans) is a bad idea. Better to extract the freebase from the toluene into acidic water using water acidified with HCL and then boil down the water solution.

Osmium

> Better to extract the freebase from the toluene into acidic water
> using water acidified with HCL and then boil down the water solution.

In my opinion that is a bad idea.
Gassing is so easy, unless you have shitloads of impurities present it will ALWAYS work. Especially with toluene. I couldn't believe it myself, but when I tried that the first time I was surprised how well it works. A toluene A/B extraction layer, not even dried with drying agent will produce beautiful white product after acetone washing (which was simply added to the toluene afterwards and gassing commenced).

terbium

I have never tried gassing in toluene, whenever I did it I used ether. So many people here seem to have trouble getting any product when gassing in toluene. I would expect HCL to be much more soluble in ether than toluene and wonder if this doesn't make a difference, especially in the dilute solutions of freebase that some people are using. Perhaps your addition of acetone to the toluene also improved the HCL solubility and thus the formation of the product.

Osmium

The big advantage of toluene is that even when it went through an A/B process, it's dry. Ether contains lots of water and has to be dried, toluene will contain much less when you sepatate the phases correctly.
Acetone doesn't make a big difference, since there's only a few percent present (none at the beginning) when you add the acetone washings to the gassing solvent. All those filtrations and washes were done in a sintered glass funnel, adding only enough acetone twice or three times to barely cover all the crystals, stirring it around with a spatula and removing it as completely as possible by drawing air through for a minute or two.
Try it out, works like a charm.

sunlight

Gassing in toluen works fine, and as Osmium says it is not necessary to dry it.
Boiling the toluene extracts adified with aq. HCl till 140 and adding acetone when temp goes down with stiring works too, but boil the aqueous acidic extracts till dryness doesn't seem a good idea, but who knows ... Probably you should get a lot of hydrated forms.

terbium


Probably you should get a lot of hydrated forms.


Methamphetamine and MDMA hydrochlorides don't form hydrates.


Osmium

At least MDMA forms several hydrates.

terbium

Really! What molar ratios of H2O to MDMA?

Chromic

PiHKAL, #109: "The actual form that the final salt takes depends upon the temperature and concentration at the moment of the initial crystallization. It can be anhydrous, or it can be any of several hydrated forms. Only the anhydrous form has a sharp mp; the published reports describe all possible one degree melting point values over the range from 148-153°C. The variously hydrated polymorphs have distinct infrared spectra, but have broad mps that depend on the rate of heating."

Merck 12th Ed: : "Properties: crystals from isopropanol/n-hexane, mp 147-148°C (Bailey). Crystals from isopropanol/ether, mp 152-153°C (Braun)."

Osmium

There used to be a page by Lamont Granquist (? or whatever his name was) at hyperreal.org, where he had collected physical data for the different MDMA hydrates. But it seems like this page is gone, all the chemistry links now go to erowid. Could be that I printed that page out a few years back, I'll have a look later today.