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Recrystalizing Mescaline HCl from 99% IPA

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w0mbat

w0mbat

Rising Star
Has anyone ever actually done this? I've heard that it works well, but do not recall reading any accounts of it actually working.

I remember someone (either bufoman or burnt) saying that this procedure was commonly used in scientific literature to purify mescaline HCl, but have been unable to find any such articles

Edit: by "recrystallize mescaline HCl from 99% IPA" I mean dissolving crude mescaline HCl in hot 99% IPA, and then placing that in the freezer to allow pure mescaline HCl to crystallize out (since it's supposedly insoluble in cold IPA)
 
ILPT just done it. A bit dissapointed he is :(

He washed very messy oily sticky brown-redish crude hydrochloride from san pedro using limo drytek with two portions of icy cold acetone (might not be 100 anhydrous) and went from 1,2g to 0,5 g :shock: :shock: :shock: Not happy at all.

Hydrochloride lost it oiliness and most of it colour became more solid, beige slightly reddish coloured clumps, still a bit sticky

He boiled this 500 mg in 30 ml of IPA(should be anhydous). He decanted the hot IPA and get 70mg of whiteish powder which hasn`t dissolved. The powder tasted salty with hint of bittersness and it was some inorganic salt (think CaCl2)

He boiled the Ipa down to 10 ml or so and put it in the freezer to precip. After 8 hours it all looked good. He had slightly reddish solution with white prec. on the bottom
Upon decantation the problems raised. the precip were tiny and still a bit sticky they also dispersed in solution which made decantation difficult. The paricles were so fine so he didn`t even think of filtering them. He lost some paricles but managed to recover 70mg of very bitter substance which is not yet clean it has this sligtly beige - pinkish colour, but it`s powdery and non sticky

Solubility of mws. hcl in IPA must be very low , because ILPT noticed that solution became cloudy and precip. formed as soon as the temerature start to drop bellow boiling point.

He has no problems with cleaning peruvianus extract prepared exactly the same way. That time he washed 3 times with acetone and twice with IPA and lost only about 30% of yield.
The solvents were from new bottles and both anhydrous. The bottles were half year old now and solvents might sucked some moisture from the air .

ILPT evaporated the washing acetone portions and then he pour in the same container and evaporated the IPA from crystalization. He ended up with brown-red oil and he try to recover more mescaline out of it but it`s gonna be pain in the arse
 
So far he can say that re-x led almost to the same leve of purity(judging by colour and consinstency) like 2-3 cold IPA washes with only difference that cold IPA washes doesn`t remove that inorganic salt.

Lost on yield with cold wash is less then wit re-x simply because solid particles aren`t as fine as one from recrystalization
 
ok, so when you dissovled the m.hcl into the ipa, was it clear, milky, colored but clear?
did you reduce volume before freezing?

if not, try this:
get hcl to dissolve, until mix is clear-even if brown or discolored, in a minimum of boiling ipa,
reduce volume by 20-50% rapid boil down is fine
if solution becomes cloudy, you have boiled enough
add 50% by volume of mek or acetone
put in freezer
pure needles grow to be filtered
 
It was transparent of red colour upon dissolving. He boiled it down until it became cloudy and stuck in the freezer for 16 hours.
He filtered off tan precip and drying them now. He has 70 mg what stucked on sides of mini beaker so far

He may try the trick of adding acetone next time , but need to dry the acetone first.
 
kemist said:
It was transparent of red colour upon dissolving. He boiled it down until it became cloudy and stuck in the freezer for 16 hours.
He filtered off tan precip and drying them now. He has 70 mg what stucked on sides of mini beaker so far

He may try the trick of adding acetone next time , but need to dry the acetone first.
Click to expand...

sweet

i've never had to dry acetone to get precip using sulphate, but hcl is a bit more water sol.
i doubt it needs to be dry anyways

how has the hcl salted? multiple washes (ie guess work) or was ph checked, ie single titration?
dark colored salts often are from a bit too much acid being used
 
dg said:
how has the hcl salted? multiple washes (ie guess work) or was ph checked, ie single titration?
dark colored salts often are from a bit too much acid being used
Click to expand...
He might used too much acid at the beginning. He doesn`t checked pH and used 10% white vinegar in first two sets of salting then he diluted the gar down to 5-6% . Following two sets of salting with diluted gar came out more pure (1 set of salting include 3 simple saltings)


From now on, he gonna be more pH aware 😉

By this washes and re-x he lost 75 % of yield from his dried san pedro outer flesh

He done 4 pulls with limo on the slightly wet basified flesh and 4 sets of salting on that filtered saturated limo to gain 2,4 g of impure acetate. He turned it to HCL salt and after all that washing and re-x he ended up with 600 mg of tanish solid hydrochloride

He still have basified flesh and limo so he`ll do another pull and will see, but so far this san pedro is dissapointing extraction.
 
For the record: you need about 8-10 ml/g of mescaline. Dissolving the crystals is quite slow and takes some time, be patient before you add more IPA.
 
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