Hydrochloric Acid → HCID 86650672, compound

Participants

Reaction Conditions

Reaction Steps

Hydrochloride Salt formation: Add concentrated HCl (2.11 mL g, 25.5 mmol) solution to a yellow solution of 4-[(3R,5R)-3-[1-methyl-1-(6-trifluoromethyl-pyridin-2-yl)-ethylamino]-2-oxo-5-(3-trifluoromethoxy-phenyl)-pyrrolidin-1-yl]-benzonitrile (10.70 g, 19.5 mmol) in ethyl acetate at 70° C. Add slowly cyclohexane (360 mL) and heat to reflux for 30 min until precipitate forms. Cool to 50° C. and stir for 2 h., then allow to stir at room temperature. Sonicate the precipitate mixture, chill in ice-bath, and filter to give 11.7 g (102% yield, undried) of 4-[(3R,5R)-3-[1-methyl-1-(6-trifluoromethyl-pyridin-2-yl)-ethylamino]-2-oxo-5-(3-trifluoromethoxy-phenyl)-pyrrolidin-1-yl]-benzonitrile hydrochloride. LC-MS ESI m/z: 549.0 (M+H)+, Tr=2.44 min., method 2.

Provenance & Evidence