反应详情

To a solution of 4-((2S)-4-((1R)-1-phenylethyl)morpholin-2-yl)benzonitrile (intermediate 9, 45.7 g, 156 mmol) in 1,2-dichloroethane (312 ml) was added 1-chloroethyl chloroformate (66.9 g, 468 mmol) at room temperature. After a reflux for 6 hours, the solution was concentrated under reduced pressure. The residue was dissolved in methanol (312 ml) and the solution was refluxed for 2 hours. After removal of the solvent under reduced pressure, the crude product was washed with acetone and dried under reduced pressure to afford 4-((2S)-morpholin-2-yl)benzonitrile hydrochloride (intermediate 10, 27.6 g, 79%).

1. temperatureAfter a reflux for 6 hours
2. concentrationthe solution was concentrated under reduced pressure
3. dissolutionThe residue was dissolved in methanol (312 ml)
4. temperaturethe solution was refluxed for 2 hours
5. customAfter removal of the solvent under reduced pressure
6. washthe crude product was washed with acetone
7. customdried under reduced pressure