反应详情

To cyclohexylthiol (23 g, 0.198 mole), a solution of potassium hydroxide (13.7 g, 0.207 mole) in ethanol (80 ml) was added dropwise at 15° C., followed by stirring at the same temperature for 24 hours. After 1-bromo-3,3-dimethyl-2-butanone (35.4 g, 0.198 mole) was added dropwise to the reaction mixture at 10°-15° C. and continued to stir at 20° C. for 5 hours, sodium tungstate (2.5 g) was added. Then, 30% hydrogen peroxide (220 g, 1.96 mole) was added dropwise at 45°-50° C. and reacted with stirring at 60°-80° C. for 30 hours. After cooling, the reaction mixture was extracted with methylene chloride (300 ml×1), the organic layer was separated, dried over anhydrous MgSO4 and evaporated to obtain 14 g of residual crude 1-cyclohexylsulfonyl-3,3-dimethyl-2-butanone as a pale yellow oil.

1. stirringto stir at 20° C. for 5 hours
2. customreacted
3. stirringwith stirring at 60°-80° C. for 30 hours
4. temperatureAfter cooling
5. extractionthe reaction mixture was extracted with methylene chloride (300 ml×1)
6. customthe organic layer was separated
7. dry with materialdried over anhydrous MgSO4
8. customevaporated