反应详情

温度

2.5 °C

A solution of (3,4-dichloro-phenyl)-methanesulfonyl chloride (500 g, 1.93 mol) and acetone (470 mL) was added over 2 h to cooled (0-5° C.), stirred concentrated ammonium hydroxide (28%, 900 mL, 227 g NH3, 13.3 mol). The reaction mixture was maintained below 12° C. during the addition. The reaction mixture was allowed to warm to room temperature and was stirred for 1 h. Water (900 mL) was added to the reaction mixture and it was stirred for 1 h. The white solid was collected by filtration, washed with cold water (2×500 mL), and vacuum dried to give 375 g (81%) of (3,4-dichloro-phenyl)-methanesulfonamide with 99% purity (as determined by HPLC).

1. temperatureThe reaction mixture was maintained below 12° C. during the addition
2. temperatureto warm to room temperature
3. stirringwas stirred for 1 h
4. filtrationThe white solid was collected by filtration
5. washwashed with cold water (2×500 mL), and vacuum
6. customdried