反应详情

Duloxetine base (99% ee, 0.5 g, 1.68 mmoles) was dissolved in acetone (5 mL) and stirred with cooling in an ice-water bath. Hydrochloric acid in diethyl ether (2M, 0.8 mL) was added, and a precipitate formed within 2 minutes. The mixture was stirred at ambient temperature 16 hours, filtered and the collected solid washed with acetone (0.5 mL). The white solid was then dried under vacuum at ambient temperature to yield duloxetine hydrochloride (0.485 g, 1.45 mmoles, yield: 86%; Chiral HPLC: 99.5% ee).

1. temperaturewith cooling in an ice-water bath
2. customa precipitate formed within 2 minutes
3. stirringThe mixture was stirred at ambient temperature 16 hours
4. filtrationfiltered
5. washthe collected solid washed with acetone (0.5 mL)
6. customThe white solid was then dried under vacuum at ambient temperature