反应详情

7.7 g (74.4 mmol) of thiomorpholine were initially charged in 100 ml of dichloromethane and, while cooling with an ice bath, admixed with 20.7 ml (15.1 g, 148.8 mmol) of triethylamine. 10.0 g (49.6 mmol) of 4-nitrophenyl chloroformate were added in portions. The reaction mixture was stirred at RT for one hour, and admixed with water and ethyl acetate. The organic phase was removed, washed with 1 N hydrochloric acid and saturated aqueous sodium chloride solution, dried over sodium sulphate, filtered and concentrated under reduced pressure. Yield: 13.2 g (99% of theory)

1. temperaturewhile cooling with an ice bath
2. customThe organic phase was removed
3. washwashed with 1 N hydrochloric acid and saturated aqueous sodium chloride solution
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure