I continue to read the post of long soaks, multiple recrystallizations, a multitude of different solvent washes and boils and evaporations. Feel free to continue doing this, all ye who have success and find ease in this, but I had an ok time extracting pseudo from some red hots with very little trouble
What I did was:
-stick all the pills (306 pills, 30mg each) and placed them in a normal margarita type blender and blended to a fine powder. The red coatings did not break up nearly even closely as well as the inside and I removed the majority of the red coatings by passing through a mesh screen with fine holes. Only a few small flakes of red remained.
-This powder was put in a flask, 125mL of 99% IPA was poured in and flask heated until near boiling for about 2 minutes. This was supernatant was filtered through very finely divided perlite to obtain a perfectly clear slightly pink solution that when somewhat below room temperature begins to precipitate.
-This was all evaporated in the sun (30 minutes or so), scraped up and placed in a flask where an ambiguous amount of toluene (sorry, roughly 100ml) was poured in and heated until near boiling then pipet-fulls of 99% IPA were added while remaining near boiling just until all of the crystals dissolved.
-This flask was then placed on a book and allowed to slowly come to room temp (tons of cotton-like crystals slowly begin to form) , then placed in the fridge and allowed to cool further (more xtals), then placed in the freezer while I prepared a buchner funnel.
-The crystals were then filtered and washed liberally with freezing cold toluene, then allowed to dry. The mass of cottonballs (5.9g) that remained were a very slight pink, with a melting point of 179-183 (theile tube).
-The crystals were dissolved in 15 mL of water and 5M NaOH was added until the pH was around 12.5-13 (crappy pH papers) to obtain a crystalline sludge.
-25mL quantities of toluene were added and stirred vigorously in an attempt to dissolve the freebase (occasionally letting the mixture settle until some of the clear non polar could be sucked off with a dropper). This took many additions of toluene (approximately >150 ml, forgive me but I did not write this down). The remaining water layer was a foggy peach color.
-The foggy toluene that was collected was filtered,dried with sodium sulphate, then evaporated in an open dish under the kitchen hood (
) to obtain 4.4g of clear colorless rectangular crystals with a melting point of 119.
(59% yield)
This was cake to perform, the only pain being evaporating the toluene. The crystals look clean as can be and are practically odorless (with a faint, and I mean faint, smell of toluene). Of course, I suspect it will lose that smell soon. I have not yet reacted using this purification product.
