反应详情

A solution of 0.642 mole of m-nitrobenzenesulfenyl chloride in enough carbon tetrachloride to make 1060 ml was prepared by passing chlorine for 6.5 hours into a solution of 99 g (0.321 mole) of bis(m-nitrophenyl)disulfide in 1 liter of carbon tetrachloride at 45° C. One-quarter of this solution (265 ml, equivalent to 0.161 mole of the sulfenyl chloride) was treated with 29.2 g (0.160 mole) of p-tolyl vinyl sulfone. Upon standing for several weeks crystals separated. Filtration gave 18 g (30%) of crude product m.p. 92°-101°. Recrystallization from 30 ml of ethyl acetate gave pure material m.p. 103.5°-104.5°.

1. customwas prepared
2. customfor 6.5 hours
3. customat 45° C
4. waitUpon standing for several weeks
5. customcrystals separated
6. filtrationFiltration
7. customgave 18 g (30%) of crude product m.p. 92°-101°
8. customRecrystallization from 30 ml of ethyl acetate