反应详情

温度

80 °C

To a mixture of 18 g of isopropyl methylsulfonylacetate, 7.6 g of carbon disulfide and 200 ml of dimethylformamide, 22.4 g of potassium hydroxide was added under ice-cooling. The resultant mixture was stirred for 2 hours. Thereafter, 13.3 g of 1,1,2-trichloroethane was added, followed by stirring at 80° C. for 3 hours. After cooling the reaction mixture, chloroform and water were added and the resulting organic layer was separated. Upon removal of the solvent by distillation under reduced pressure, 24.1 g of the title compound was obtained as pale yellow crystals. Upon recrystallization from isopropanol, they turned to white crystals. Melting point: 127°-127.5° C.

1. additionwas added under ice-
2. temperaturecooling
3. additionwere added
4. customthe resulting organic layer was separated
5. customUpon removal of the solvent
6. distillationby distillation under reduced pressure