p-Toluenesulfonic acid → Dactolisib tosylate

Participants

Reaction Conditions

Reaction Steps

2-methyl-2-[4-(3-methyl-2-oxo-8-quinolin-3-yl-2,3-dihydro-imidazo[4,5-c]quinolin-1-yl)-phenyl]-propionitrile (compound of formula I) is dissolved in formic acid at 56° C. and the resulting solution is clear filtered. The filtrate is then concentrated and a solution of p-toluenesulfonic acid (1.05 eq) in acetone is added within 30 minutes. After 25% and 50% of the addition volume, the mixture is seeded to initiate crystallization. A further amount of acetone is added and the suspension is cooled down to 0° C. The crystallized product (form A of compound I monotosylate) is collected by centrifugation and dried at 60° C. under vacuum.

Provenance & Evidence