反应详情

3-(2-Chloro-4-trifluoromethylphenylsulfonyl)-1,2,4-triazole (3.12 g) and diethyl carbamoyl chloride (1.62 g) are dissolved in pyridine (10 ml) and reaction is performed at 50° C. for 5 h. After completion of the reaction, water (50 ml) is added to the reaction solution and the reaction product is extracted twice with ethyl acetate (100 ml). The ethyl acetate layer is washed first with 1N HCl, then with water, and subsequently dried with magnesium sulfate. The dried product is concentrated to form a crystal. Recrystallization from benzene/n-hexane produces the titled compound, 1-(diethylcarbamoyl)-3-(2-chloro-4-trifluoromethylphenylsulfonyl)-1,2,4-triazole, in an amount of 3.80 g; yield, 92.5%; m.p. 105.5°-107° C.

1. customreaction
2. additionis added to the reaction solution
3. extractionthe reaction product is extracted twice with ethyl acetate (100 ml)
4. washThe ethyl acetate layer is washed first with 1N HCl
5. dry with materialwith water, and subsequently dried with magnesium sulfate
6. concentrationThe dried product is concentrated
7. customto form a crystal
8. customRecrystallization from benzene/n-hexane