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Converting FB to fumerate question - Pure MgSo4, no need to oven? Can ethanol be used as solvent?

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R

Rush56

Ruzhxy
Hi.

I decided to make some fumerate salts, so i can store it for long time and when needed convertt back to FB. Or maybe use for oral route once i might be ready.

Now i wonder about "anhydous acetone".

I bought supposedly pure aceton, but cannot find any data sheets. Reading here how to make it anhydous, i bought magnesium sulphate. It is noted it is pharmacutically clean.
Now i asked the supplier whather this is heptahydrate or actually MgSo4 and they said it is MgSo4, magnesium sulphate.

Other shops do sell heptahydrate mostly.

So considering it is supposedly not a heptahydrate i assume i do not need to put it into oven?

Another question is, could i also use 96% ethanol with addition of sulphate to dry it out instead of acetone? I havent opened the can yet and tested, evaporated it to confirm it is clean, so in case it wouldnt be, would ethanol work?

While one can drink ethanol, diluated i prefer to use it when i can. I was always a bit scared of acetone, not sure why and i never used it before.
 
Hmm? So just use plain acetone? Why all that talk about anhydous acetone in all teks i found?

In case of ethanol, i should dry it using MgSo4? There is 4% water, which is not good right? Will it percipitate normally in ethanol?

I am a bit confused as most teks seem pretty old, which one should i follow for optimal results for dmt fumerate? Which is the best up-to-date tek?
 
Ethanol does not dry well with MgSO4. There are a number of treatises on drying methods for various solvents which should be required reading.

DMT fumarate has a somewhat lower solubility in isopropanol than in ethanol. I've successfully dried IPA to an unmeasured extent using anhydrous sodium carbonate. You can't use sod.carb for acetone, by the way.

There's a bit of an argument about how significant the aldol condensation with MgSO4 and acetone is. Minimization of contact time is obviously desirable if you have no other alternative, but it should be easy enough to find (or make) sodium sulfate which is significantly less acidic. It's also worth noting that molecular sieves promote the aldol condensation even more than MgSO4 does (from what I've read, iirc) - and anhydrous acetone by itself is said to form aldol condensation products spontaneously anyhow.
 
downwardsfromzero said:
Ethanol does not dry well with MgSO4. There are a number of treatises on drying methods for various solvents which should be required reading.

DMT fumarate has a somewhat lower solubility in isopropanol than in ethanol. I've successfully dried IPA to an unmeasured extent using anhydrous sodium carbonate. You can't use sod.carb for acetone, by the way.

There's a bit of an argument about how significant the aldol condensation with MgSO4 and acetone is. Minimization of contact time is obviously desirable if you have no other alternative, but it should be easy enough to find (or make) sodium sulfate which is significantly less acidic. It's also worth noting that molecular sieves promote the aldol condensation even more than MgSO4 does (from what I've read, iirc) - and anhydrous acetone by itself is said to form aldol condensation products spontaneously anyhow.
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Hmm ok now i am even more confused, its somewhat hard for me to understand all this. So what do you suggest?

Am i better staying with FB and storing in fridge in airtight glass jars? Ive noticed that at room temps white snowy xtals turned somewhat yellowish a bit goey after months...

Edit: The IPA route is not sounding too nice to me, when i was looking in best ways to make canna oil there was a lot of talk of IPA being unhealthy with such teks..
 
My suggestion: Forget magnesium sulphate or any chemical drying of acetone for your case. Chances are your acetone is already dry enough to do FASA. If for some unlikely reason your acetone was too wet and your fumarates did not crash out, you could try putting it in the fridge and see if they do crash. And even if not, you can always evap your acetone and you´ll have a mix of excess fumaric acid with your DMT fumarate, and then you can use any number of ways to recover your actives and separate them from your excess fumaric acid
 
endlessness said:
My suggestion: Forget magnesium sulphate or any chemical drying of acetone for your case. Chances are your acetone is already dry enough to do FASA. If for some unlikely reason your acetone was too wet and your fumarates did not crash out, you could try putting it in the fridge and see if they do crash. And even if not, you can always evap your acetone and you´ll have a mix of excess fumaric acid with your DMT fumarate, and then you can use any number of ways to recover your actives and separate them from your excess fumaric acid
Click to expand...

Nice. I may give it a shot with small batch.

What about losses if one starts lets say with 100mg, turned to fumerate and back to FB, what to expect?
 
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