反应详情

m-Chlorobenzamide (75 g, 0.48 mol) and chlorocarbonylsulfenyl chloride (79 g, 0.6 mol, 25% excess) were reacted as described in Example 2 for 1.5 hours. Volatile components were removed under reduced pressure. The dark brown oil was taken up in hot cyclohexane, and the mixture was filtered. Cooling resulted in separation of a dark orange solid. The solid, recrystallized twice from hot ethyl acetate, gave 64.21 g (0.316 mol, 65.8%) of off-white solid, m.p. 83+-84.5°.

1. customVolatile components were removed under reduced pressure
2. filtrationthe mixture was filtered
3. temperatureCooling
4. customresulted in separation of a dark orange solid
5. customThe solid, recrystallized twice from hot ethyl acetate