|LSA - Crystals dammit!||Bookmark|
Ok, SWIP's an impatient little bastard, I've tried to tell him to calm but he won't. So in between 12 hour shifts spent waiting by the letterbox for his seeds, he insists on sharing his procedure proposal with you to look for flaws.
SWIP wants crystals, yes he's fastidious as well as impatient. But frankly, while yellow gunk in gelcaps is good enough for an ageing tree-dwelling hippy named 'Daisy', SWIP will have nothing of the sort. Its crystals all the way, and the purer the better.
So here goes:
1) Grind into powder. (Seeds are not coated)
2) Non-polar soak.
3) Polar Soak.
4) HCl Soak.
5) Activated charcoal boil.
6) Vacuum filter.
7) Finish A/B extraction to obtain freebase.
8) Dissolve in hot, dry MeOH, add tartaric acid & Et2O ala. Shulgin to form tartrate salt and recrystallise.
9) Repeated recyrstallisation until crystals are virtually insoluble.
Should bee sufficient ?!
|you need chromatography||Bookmark|
I've never done it, but I would expect that you need several chromatographic steps to get a crystalline product.
SWIM has used idiotically simple base-precipitation from polar (tea) to yield nice, clean, tasty alkaloid in the coffee filter.
THAT much don't take... that much.
Now, if one wants a finely hand-grown crystal of pure ammonium lysergate, one's going to have a bit more of a bitch of a time...
...do everything under helium in the freezer. Chromatograph. Use freezing point variance to test the mol. wt. of each flourescent band. Do your own math, take the one you want, and from there...
...well, I'm not sure WHAT would best recrystallize ammonium lysergate at 0c, but probably near-anything with a good vacum to evap... ::shrug:: It's chromatographically cleansed already, right?
Choice is yours. Quick-'n-easy precipitate does just lovely.
'course, so does quick-'n-easy lemonade...
Edit : coming back to this later, I note that you say
Activated charcoal boil.
Boil? BOIL??!!?! You'd BEST be talkin' at DARN cold temperature, under vacum - 'cause I reckon there's a LOT of people here against drug abuse... and boiling ergot alkaloids would DEFINATELY be abusive to 'em.
These things THERMALLY DEGRADE... EASILY...
Anyways, to go over this while paying a bit more explicit attention...
3) Polar Soak.
Base first, if you do this (Umm... AFTER step 2). Most organic matter is lightly acidic, for the obvious reasons (ugh... crack... rock... precipitated... in... brain.... now... having... stroke...).
Anyways, aside from these points, you've gone beyond 'sufficient' into 'overkill' - I would not be surprised in the slightest if, should you match the HCl solution with the expected alkaloidal yield fairly well, you would be performing unneccesary steps on a vial of LSxA HCl.
'course, overwash was never a bad thing. Considering, though, I'd either skip the charcoal step entire (it likes to grab polarish stuff, alkaloids inclusive at times - with nothing else to work with, it's just grabbing yer LSxA HCl salts - though it might take a detour to form DCM with any excess HCl).
For the most part, though, mad props - overwashing never hurt anything...
Oh - and you might not want to rule out chromatographing yer product, since you're a purity nut. Name each of the flourescent bands, and see which does PRECICELY what to yer head. :) If you find any interesting variants, take the mol. wt. of a sample of each, k? I've been debating doing the research for some time now, for the good of science, humanity, and wingnut curiosity...
And - just to make sure yer head comes back - have a mind to dosage, k? As amusing as it would be to read in the paper 'individual eats 5g of ergot alkaloids,' it'd kinda cut down the coherency of your posting a tad...
...err... I'll stop editing now. :)
Rev. Psi Locybe, insane alchemist.