反应详情

150 ml of benzene was added to 5.0 g of N-(1-hydroxy-2,2,2-trichloroethyl)nicotinamide. 2.6 g of thionyl chloride was added dropwise to the mixture under stirring. Then, the mixture was heated under reflux (60° to 80° C.) for about 5 h to complete the production of N-(1,2,2,2-tetrachloroethyl)nicotinamide. The reaction liquid was cooled to 30° C. or below and 1.7 g of sec-butylmercaptan was added thereto. 3.7 g of triethylamine was added dropwise to the liquid mixture while it was kept at 5° C. The obtained mixture was stirred at room temperature for 3 h and then left to stand at room temperature overnight. The reaction liquid was poured in an aqueous sodium bicarbonate solution and a benzene layer thus separated was washed with a saturated aqueous common salt solution and water and then dried over anhydrous sodium sulfate. After concentration, the residue was recrystallized from a solvent mixture of n-hexane and ethyl acetate to obtain 2.5 g of N-(1-sec-butylthio-2,2,2-trichloroethyl)nicotinamide.

1. temperatureThen, the mixture was heated
2. temperatureunder reflux (60° to 80° C.) for about 5 h
3. customThe reaction liquid
4. temperaturewas cooled to 30° C. or below
5. customwas kept at 5° C
6. stirringThe obtained mixture was stirred at room temperature for 3 h
7. waitleft
8. customThe reaction liquid
9. customa benzene layer thus separated
10. washwas washed with a saturated aqueous common salt solution and water
11. dry with materialdried over anhydrous sodium sulfate
12. concentrationAfter concentration
13. customthe residue was recrystallized from a solvent mixture of n-hexane and ethyl acetate