反应详情

In a 100 ml Fisher-Porter pressure vessel were placed 9.0 g (0.024 mol) of 4-(2,2-dichloro-1,1-difluoroethoxy)-2-methyl-5-nitrobenzenesulfonyl chloride, 2.4 g (0.048 mol) acrylonitrile, 2 ml acetonitrile, 0.07 g cupric chloride and 0.12 g triethylamine hydrochloride. After cooling and evacuating the vessel to 5 mm mercury pressure, it was sealed and heated in an oil bath at 105°-110° C for 38 hours. The vessel was opened and the reaction medium was filtered with the aid of benzene. The insolubles were discarded and the filtrate was treated with 5.0 g of triethylamine, refiltered, and washed with water. After decolorizing wth charcoal and drying over MgSO4, removal of the solvent under reduced pressure afforded a dark amber oil. Recrystallization from methanol provided 1.0 g of the title compound as a white solid, m.p. 109° C.

1. temperatureAfter cooling
2. customevacuating the vessel to 5 mm mercury pressure, it
3. customwas sealed
4. temperatureheated in an oil bath at 105°-110° C for 38 hours
5. filtrationthe reaction medium was filtered with the aid of benzene
6. additionthe filtrate was treated with 5.0 g of triethylamine
7. washwashed with water
8. dry with materialdrying over MgSO4, removal of the solvent under reduced pressure
9. customafforded a dark amber oil
10. customRecrystallization from methanol