反应详情

Hydrogen peroxide (30%, 100 ml) was added to a stirred mixture of 4-(N,N-dimethylaminosulphonyl)-2-trifluoromethylbenzonitrile (20.37 g) and sodium hydroxide (1.0 g) in ethanol under an inept atmosphere maintaining the temperature at 40°-45° C. The mixture was stirred and heated at that temperature for 3.5 hours. It was cooled, poured into water, sodium chloride was added and it was extracted with ethyl acetate, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was re-crystallized from a mixture of ethyl acetate and toluene to give 4-(N,N-dimethylaminosulphonyl)-2-trifluoromethylbenzamide (16.44 g) as white crystals, m.p. 149°-156° C.

1. temperaturemaintaining the temperature at 40°-45° C
2. temperatureheated at that temperature for 3.5 hours
3. temperatureIt was cooled
4. additionwas added
5. extractionit was extracted with ethyl acetate
6. washwashed with water
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customThe filtrate was evaporated to dryness
10. customthe residue was re-crystallized from a mixture of ethyl acetate and toluene