反应详情

3.1 g of ethanesulfonamide was dissolved in 50 ml of dry tetrahydrofuran, and 1.2 g of 60% sodium hydride was added thereto under cooling with ice. After completion of the addition, the mixture was reacted for one hour under reflux. After cooling, 5.0 g of 2-chloro-3-nitro-5-trifluoromethylpyridine was added thereto, and then the mixture was reacted for 7 hours under reflux. After completion of the reaction, the reaction product was poured into 200 ml of water. Undissolved materials in water were extracted with ethyl ether and removed. Then, the aqueous layer was weakly acidified with dilute hydrochloric acid. Precipitated crystals were collected by filtration and dried to obtain 3.6 g of N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide having a melting point of from 160° to 163° C.

1. temperatureunder cooling with ice
2. additionAfter completion of the addition
3. customthe mixture was reacted for one hour
4. temperatureunder reflux
5. temperatureAfter cooling
6. customthe mixture was reacted for 7 hours
7. temperatureunder reflux
8. customAfter completion of the reaction
9. extractionUndissolved materials in water were extracted with ethyl ether
10. customremoved
11. customPrecipitated crystals
12. filtrationwere collected by filtration
13. customdried