HRID1089787

反应详情

EQUATION

反应方程式

HRID 1089787 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-chloroperoxybenzoic acid (3.49 g) in dichloromethane (80 ml) was added to a stirred solution of 1-(4-fluoro-2-methylaminophenyl)-2-(methylthio)ethanone (4.3 g), prepared in a similar manner to that described in Example 2, in dichloromethane (75 ml) under nitrogen over 15 minutes whilst maintaining the temperature below 25°. The mixture was stirred for a further 2 hours at ambient temperature. The solution was washed with saturated aqueous sodium hydrogen carbonate solution (3×50 ml) and evaporated in vacuo to give a solid product. Crystallisation from toluene gave 1-(4-fluoro-2-methylaminophenyl)-2-methylsulphinylethanone, m.p. 137°-138°.

WORKUP

后处理

  1. customprepared in a similar manner to that
  2. temperaturewhilst maintaining the temperature below 25°
  3. washThe solution was washed with saturated aqueous sodium hydrogen carbonate solution (3×50 ml)
  4. customevaporated in vacuo
  5. customto give a solid product
  6. customCrystallisation from toluene