Author Topic: sulfate salt?  (Read 1389 times)

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abc123

  • Guest
sulfate salt?
« on: July 14, 2001, 03:23:00 AM »
instead of gassing ...32%HCl can be dripped onto a product but the water will dissolve it and it will take forever for crystals to form
 but is it possible to take a few drops of 96% H2SO4 and dilute with DCM and pour that directly onto your oil and make a sulfate...would this work?

b159510

  • Guest
Re: sulfate salt?
« Reply #1 on: July 14, 2001, 07:28:00 AM »
I think that for sulfuric acid to fully dissociate, it
should be diluted w/ water to a max concentration of
~ 10%. Some sulfate salts of amines are soluble in DCM.

AMINATOR

  • Guest
Re: sulfate salt?
« Reply #2 on: July 14, 2001, 07:34:00 AM »
I heard the best way to do that is to disolve your freebase in acetone and drip in your 95-99% sulphuric and the salt precipitates. the acetone and any water will form a solution but the acetone will still maintain a good solubility barrier especially scince there hardly any water in the acid. after you filter you product placing the tone in the freezer should get you any that did dissolve but it won't be much if any. happy cookin!  :)

b159510

  • Guest
Re: sulfate salt?
« Reply #3 on: July 14, 2001, 08:58:00 AM »
Has any bee used this acetone/conc.sulfuric acid method
to form the sulfate salt of an amine? I have not heard
of this, and it seems the reaction between acetone and
conc. sulfuric acid would be undesirable.

Rhodium

  • Guest
Re: sulfate salt?
« Reply #4 on: July 14, 2001, 04:13:00 PM »
Yes, better use diethyl ether instead of acetone when doing this. The acid could catalyze imine formation between the amine and acetone.


https://www.rhodium.ws


Osmium

  • Guest
Re: sulfate salt?
« Reply #5 on: July 15, 2001, 01:27:00 AM »
I don't like such "shortcuts" at all. When done correctly this even might be a good way to crystallize, but my experience tells me that most bees using this route will end up with an unstable dirty product. Same goes for that "add HCl to freebase and let evaporate" method. Bad chemistry IMHO.
What is wrong with gassing? Works every time. If your product doesn't crystallize then it's very impure and you obviously didn't do an A/B, in which case you deserve to end up with peanut butter anyway, for being too lazy to do this easy and highly efficient step.

AMINATOR

  • Guest
Re: sulfate salt?
« Reply #6 on: July 15, 2001, 02:21:00 AM »
yeah, Ive always just gassed it myself, that method is from pugsleys pseudonitrsite text on rhodiums site...I assumed it was legit. gassing is easy. if you don't want to do a reaction. you can also just bubble air though it and dry the gas with calcium chloride or something...or maybe a reaction is better. Ive had good results with gas by this method but have never used a Nacl+H2so4 reaction yet.

Scooby_Doo

  • Guest
Re: sulfate salt?
« Reply #7 on: July 15, 2001, 03:07:00 PM »
Sulfuric acid is insoluble in DCM. Making good crystals with H2SO4 is just as much work as gassing with HCl like Os hinted. However there was a post on the old board who crystalized MDA in ethanol using sulfuric acid which worked well. I can't remember if it was conic or diluted a little.

AMINATOR

  • Guest
Re: sulfate salt?
« Reply #8 on: July 17, 2001, 01:57:00 AM »
I would probably dilute to at least half probly less. Just safer to judge dropwise. also I guess the product will decompose if excess acid is left on it.recystalisation from a miniumum amount of hot methanol is recomended after making the sulphate.put it in the freezer.


endo1

  • Guest
Sulfate w IPA
« Reply #9 on: June 18, 2002, 07:13:00 AM »
SW likes to turn MDA in to MDA sulfate when his batches are 1/2 kg+. SW has been diluting 99% H2SO4 w 99% IPA to make a 10% H2SO4 solution (No water). Not sure why boiling the H2SO4 solution or adding water was suggested earlier in this thread but he does not do that. He uses IPA (7x volume of base) w base disolved in it then SLOWLY adds dilute H2SO4 solution with lots of stirring. He watches PH with a hydroponic PH pen. He is very carefull not to go below 8. SW is not sure what exactly happens when filtered while PH is below 8 but he has heard some nasty rumors about product turning color/ turning to mush. Best thing to do if PH < 8 is to add more base so always hold back a bit of base. SW thinks that many other solvents could replace the IPA in the above procedure.

SW thinks that the sulfate anion is divalent so 1 sulfate anion attaches to two MDA molecules to make one molecule. That would mean MDA sulfate has a molecular weight of 454.5 and is twice as strong as 1 HCl salt molecule (weight = 215.68). 1g of MDA base should make 1.2680017g of MDA sulfate(or 1.2034438g of MDA Hcl). If SW's above calculations are correct then a slight adjustment to dosage is in order if you were using the HCl salt before. For instance if you considered 1 dose of MDA HCl to be 80mg then 1 dose of the sulfate would be about 84.2mg.

SW's sulfate product seems to be whiter, friendlier to the nose, less hygroscopic and it seems to have much less smell than his HCl salt product. (Note: he does use hardware store toluene when he makea his HCl product.)

endo1

  • Guest
Uh oh, when using the above procedure SW has ...
« Reply #10 on: July 19, 2002, 09:53:00 PM »
Uh oh, when using the above procedure SW has noticed only 80-90% of product recovered (SOME of the missing product IS recovered as base if 2x volume of water added to remaing solvent and another A/B is done). Could this be from the 1 or 2% water in the IPA or H2SO4? 99% lab grade IPA and 98% lab grade H2SO4 were used. He has also tried brining the Ph down to 7 while filtering lots through out the procedure(this seemed to get the best yield but still only <90%. Also a little more product does ppt going from Ph 8 to 7). After the first patty is filtered product DOES show signs of water present (sticks to filter paper and plugs it up, slow flowing solvent thru product etc.) SW also noted that 10 to 15% more H2SO4 was required to bring the PH to the desired level than was calculated by the mol math. (pure distilled MDA base was used) Is MDA sulfate a little bit soluble in IPA? Is H2O created during this method of crystalization? If not where does the H2 go? Can MgSO4 be used to dry IPA/Base and or IPA/H2SO4 before procedure is started? (and would this help?) Should he try using toly or ether instead of IPA?



Osmium

  • Guest
The reason is that you add H2SO4 until you reach ...
« Reply #11 on: July 19, 2002, 11:23:00 PM »
The reason is that you add H2SO4 until you reach pH 8. That is clearly not enough H2SO4

I'm not fat just horizontally disproportionate.

endo1

  • Guest
Thanks O
« Reply #12 on: July 26, 2002, 12:36:00 AM »
Thanks O but I did mention SW went to pH7 and didn't get much more pcpt. He did find his missing product after distilling the solvent away he was left with a significant mass of brown crud. A small sample of this brown crud disolved in IPA! A sample of his original filtrate (MDA-SO4) did not. SW thinks some MDA bisulfate compound was formed by acdident. bisulfate was reacted with naoh solution to give back base and product recrystalized via HCl. SW thinks he needs to add the H2SO4 solution way fucking slower. Any other hints on preventing the bisulfate from forming? cooling perhaps?

neuromodulator

  • Guest
Crystallization.
« Reply #13 on: July 27, 2002, 08:10:00 PM »
There are 1001 ways to skin a cat.  Also, it depends on the cat in question.