SWIM decided to do another trial, preparing a snortable salt.
100 mg. freebase was dissolved in a minimum amount of IPA in a test tube (some heating applied), one drop 96% H
2SO
4 was added, and after the solution returned to RT, an equal volume of acetone was added.
The test tube was cooled in the freezer, and after 3 hours nothing had precipiated.
Another experiment was perfomed...
250 mg. freebase was dissolved in a minimum amount of acetone (again some heating was applied).
2 drops of 96% H
2SO
4 was added, which resulted in a pop & hizz and
instant crashing of the sulphate salt.
After a few seconds, the salt had settled to the bottom - then gravity filtered and dried, yielding 175 mg. of fine-snowwhite powder.
SWIM used to much acetone (and not 100% anhydrous solvents), which without doubt was the main reason for the low yield.
Conversion from the freebase to the dry sulphate took about 10-15 minutes, and instant bio-assay (
) proved IN-administration indeed effective!
(Guess who haven't slept tonight?
)
Bees, this is the salt of your choice!
SWIM might try recrystallizing in a dual solvent system (IPA/EtOH + Acetone) in near future.
...sorry 'bout potential grammatic errors, i need sleep!