(±)-Bis-tetralone (BisT) crystallizes
as a stable conglomerate
that can be resolved by preferential crystallization. This preferential
crystallization was performed by autoseeded polythermic programmed
preferential crystallization (AS3PC) and autoseeded preferential crystallization
induced by solvent evaporation (ASPreCISE) variants in dimethylformamide
and dichloromethane. Prior to performance of these resolutions, an
extensive purification was necessary because the presence of impurities
had a strong negative impact on the stereoselective crystal growth.
Moreover, the presence of multiepitaxy phenomena required a vigorous
stirring during the preferential crystallization in order to avoid
a poor optical purity of the crops. Several preferential crystallization
attempts demonstrate that ASPreCISE is recommended when there is an
unfavorable variation of solubility versus temperature or when chemical
degradation occurs on heating.