反应详情

To a solution of 42.2g (0.2 mole) 4-(4-chlorophenyl)urazole in 200 ml water was added a solution of 16g (0.4 mole) sodium hydroxide in 20 ml water. A mixture of 74.4g (0.4 mole) trichloromethylsulfenyl chloride and 3g of an emulsifier solution (as in example 1) in 50 ml water was added dropwise to the above basic solution while keeping the reaction mixture at 0° C. The reactants were mixed so that the reaction mixture was kept at a pH greater than 7. The precipitate that was formed was collected on a filter and the filter cake was washed with water. After drying, triturating with ethyl ether, and recrystallizing from benzene-cyclohexane (1:1, by volume) there was obtained 42g (64%) of 4-(4-chlorophenyl)-1, 2-bis(trichloromethylthio)urazole having a melting point of 169° C.

1. additionwas added dropwise to the above basic solution
2. customat 0° C
3. additionThe reactants were mixed so that the reaction mixture
4. customThe precipitate that was formed
5. customwas collected on
6. filtrationa filter
7. washthe filter cake was washed with water
8. customAfter drying
9. customtriturating with ethyl ether
10. customrecrystallizing from benzene-cyclohexane (1:1, by volume) there