p-Toluenesulfonic acid monohydrate → HCID 86650871, compound

Participants

Reaction Steps

Dissolve (3R,5R)-3-[1-methyl-1-(2-trifluoromethyl-pyrimidin-4-yl)-ethylamino]-5-(3-trifluoromethoxy-phenyl)-1-(4-trifluoromethyl-phenyl)-pyrrolidin-2-one (4.57 g, 7.71 mmol) in isopropanol (10 mL). Add p-toluenesulfonic acid monohydrate (1.49 g, 7.71 mmol) and heat to 45° C. until the solution is homogeneous. Cool to ambient temperature and add seed crystals. Let stand at ambient temperature for 64 hours. Filter the precipitate and wash with heptane. Dry under vacuum for 4 hours to give (3R,5R)-3-[1-methyl-1-(2-trifluoromethyl-pyrimidin-4-yl)-ethylamino]-5-(3-trifluoromethoxy-phenyl)-1-(4-trifluoromethyl-phenyl)-pyrrolidin-2-one tosylate (5.06 g, 86%) as a white powder. LC-MS ESI m/z: 593 (M+H)+, Tr=4.92 min., method 1.

Provenance & Evidence