反应详情

Using the method of Example 3, a mixture of 1-trifluoromethylthio-2-propanone (0.15 mole), dichloromethane (75 ml), ethanol (0.3 g) and trifluoromethanesulfenyl chloride was loaded into a sealed metal reaction vessel. The reaction was carried out for 67 hours at room temperature. Most of the dichloromethane was removed by distillation. Vapor phase chromatography of the residual liquid showed about 55 percent unreacted 1-trifluoromethylthio-2-propanone and two products. The distillation residue was returned to the sealed metal reactor, 11.2 g (0.082 mole) of trifluoromethanesulfenyl chloride and 75 ml of dichloromethane were added, and the reaction was allowed to continue for 12 days at room temperature. The dichloromethane was removed by distillation and the residue was examined by vapor phase chromatography. This analysis showed only 16% unreacted starting material. Fractional distillation of the reaction mixture gave 1,1-bis(trifluoromethylthio)-2-propanone, b.p. 44°C/23 mm Hg and 1,3-bis(trifluoromethylthio)-2-propanone, b.p. 67°C/5 mm Hg. These structures were established by elemental and spectral analyses.

1. customwas loaded into a sealed metal reaction vessel
2. customMost of the dichloromethane was removed by distillation
3. additionwere added
4. waitto continue for 12 days at room temperature
5. customThe dichloromethane was removed by distillation
6. distillationFractional distillation of the reaction mixture