HRID129375

反应详情

EQUATION

反应方程式

HRID 129375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 2-propanethiol (12.2 g, 0.16 mole), a solution of potassium hydroxide (11.5 g, 0.174 mole) in ethanol (100 ml) was added dropwise at 15° C. or lower, and continued to stir at the same temperature for 24 hours. Then chloroacetone (23.1 g, 0.25 mole) was added dropwise at 10°-15° C., and reacted with stirring at 20° C. for 4 hours. To this mixture, sodium tungstate (0.8 g) was added, 30% hydrogen peroxide (36 g, 0.32 mole) was added dropwise at 45°-55° C., and reacted with stirring at room temperature for 14 hours. The reaction mixture was extracted with methylene chloride (200 ml). The organic layer was washed with H2O, dried over anhydrous MgSO4 and evaporated to give 18.9 g of residual crude 1-(1-methylethylsulfonyl)acetone as a brownish yellow oil.

WORKUP

后处理

  1. customreacted
  2. stirringwith stirring at 20° C. for 4 hours
  3. customreacted
  4. stirringwith stirring at room temperature for 14 hours
  5. extractionThe reaction mixture was extracted with methylene chloride (200 ml)
  6. washThe organic layer was washed with H2O
  7. dry with materialdried over anhydrous MgSO4
  8. customevaporated