I did a set of microscale isopropanolic recrystallization trials on some clean mixed harmala hydrochloride dihydrate [manske crystals].
In boiling 99% isopropanol I produced 16ml of a 0.8% solution and on cooling to -10°C I recovered 59% of the alkaloid as crystals. Given the large volume that would be needed, and the poorer crystal formation, I dont like 99% IPA.
In near-boiling 91% isopropanol I produced 12ml of a 2.9% solution and on cooling to -10°C I recovered 83% of the alkaloid as crystals.
The microscale work might have harmed recovery a little bit, particularly since I didnt have vacuum filtration. Larger batches should see a marginal to moderate improvement in yield. Another limiting factor is I dont know if some of the water of hydration may have been lost in the recrystallization. Isopropanol forms an azeotrope with water so boiling could have driven some water off, as 87.4% isopropanol boils lower than 99% IPA. Its also unknown how hard harm[al]ine tries to grab onto water as it crystallizes from organic solvents.
The commonly available 91% IPA seems a feasible solvent for recrystallization.
Procedure employed:
A measured amount of alkaloid was placed into hot solvent
This beaker was placed in a hot water bath and stirred for several minutes while being maintained at or near boiling
The solution was then carefully decanted off the remaining solids and its volume measured while the beaker containing the undissolved solids was placed in a 35°C location to air dry for measurement
The hot solution was allowed to cool first at room temperature, then at 4°C, then at -10°C
After crystallization was complete the mixture was filtered through a weighed filter paper, with the beaker being rinsed of residual crystals with some of the filtered solution
The filter containing the crystals was gently squeezed to get out most remaining liquid, and then it was pressed in a paper towel to remove as much liquid as possible
The filter was placed in an open petri dish in a 35°C location to dry and it was then weighed