HRID453118

反应详情

EQUATION

反应方程式

HRID 453118 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 2-(benzyloxy)-4-chlorobenzamide (0.103 g, 0.38 mmol) in toluene (5 ml) was added chlorocarbonylsulfenyl chloride (63 μL, 0.76 mmol) under nitrogen atmosphere and the resulting reaction mixture was refluxed at 90° C. for 2 h. After the completion of the reaction (TLC monitoring) water was added followed by extraction with ether (3×25 ml). The combined organics was then sequentially washed with water, 10% NaHCO3 (aqueous solution) and finally again with water. The organic layer was then dried over anhydrous Na2SO4, filtered and concentrated to get desired product (0.12 g, 94%) that was carried forward as such without further purification. MS: 320.21 (M+H)+.

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. additionwas added
  3. extractionfollowed by extraction with ether (3×25 ml)
  4. washThe combined organics was then sequentially washed with water, 10% NaHCO3 (aqueous solution) and finally again with water
  5. dry with materialThe organic layer was then dried over anhydrous Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated