反应详情

The clear solution of 3-trifluoromethyl-4-chloroaniline (45 g, 0.230 mol) and pyridine (37 ml, 0.460 mol) in dichloromethane (450 ml) cooled at 0° C. to −5° C. and a solution of trichloroacetyl chloride (31 ml, 0.2876 mol) in dichloromethane (100 ml) was added drop wise maintaining temperature of the reaction mass below 0° C. The reaction mass was then stirred for 1 hour below 0° C. and quenched with water (250 ml) below 5° C. The organic phase was separated and aqueous layer was re-extracted with dichloromethane. The combined dichloromethane layer was washed with water, dried over sodium sulfate and evaporated under vacuum to obtain (62 g) of the desired product, i.e., 2,2,2-trichloro-N-(4-chloro-3-(trifluoromethyl)phenyl)acetamide.

1. temperaturewise maintaining temperature of the reaction mass below 0° C
2. customquenched with water (250 ml) below 5° C
3. customThe organic phase was separated
4. extractionaqueous layer was re-extracted with dichloromethane
5. washThe combined dichloromethane layer was washed with water
6. dry with materialdried over sodium sulfate
7. customevaporated under vacuum