反应详情

(R)-7-[3-tert-Butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine-1-carboxylic acid isopropyl ester 35a (0.17 g, 0.29 mmol) and 10 mL of ethyl acetate were added into the reaction flask. A solution of 5.5 N hydrochloric acid in 5 mL of ethyl acetate was then added to the reaction flask in an ice-water bath. Upon completion of the addition, the ice-water bath was removed. The reaction mixture was stirred at room temperature for 2 hours and monitored by thin layer chromatography until the disappearance of the starting materials. The reaction mixture was concentrated under reduced pressure, and washed with n-hexane (10 mL×2). The filtrate was concentrated under reduced pressure to obtain the title compound (R)-7-[3-amino-4-(2,4,5-trifluoro-phenyl)-butyryl]-3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine-1-carboxylic acid isopropyl ester hydrochloride 35 (0.15 g, yield 97.8%) as a white solid.

1. additionUpon completion of the addition
2. customthe ice-water bath was removed
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. washwashed with n-hexane (10 mL×2)
5. concentrationThe filtrate was concentrated under reduced pressure