反应详情

温度

25 °C

A 4.0 g (0.04 mol) sample of triethylamine was added dropwise to a cooled (-10° to 0° C.) solution of 9.5 g (0.0324 mol) N-(cyclohexyl)trichlorovinylsulfonamide, m.p. 152°-153° C., and 7.6 g (0.0324 mol) 1,1,2,2-tetrachloroethylsulfenyl chloride in 200 ml dichloromethane. The reaction mixture was then stirred at about 25° C. for 3 hours, washed with water, dried over magnesium sulfate and evaporated to give an oil. The oil was chromatographed on silica gel. The N-cyclohexyl-N-(1,1,2,2-tetrachloroethylthio)trichlorovinylsulfonamide product, 11 g (72% yield), was eluted from the silica gel with 30% ether/20% hexane. The infrared spectrum of the product showed strong absorption bands at 1385 cm-1 and 1160 cm-1. The elemental analysis for the product is tabulated in Table I under Compound No. 6.

1. washwashed with water
2. dry with materialdried over magnesium sulfate
3. customevaporated
4. customto give an oil
5. customThe oil was chromatographed on silica gel
6. washThe N-cyclohexyl-N-(1,1,2,2-tetrachloroethylthio)trichlorovinylsulfonamide product, 11 g (72% yield), was eluted from the silica gel with 30% ether/20% hexane
7. customabsorption bands at 1385 cm-1 and 1160 cm-1