HRID2399781

反应详情

EQUATION

反应方程式

HRID 2399781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 4-chloro-2-(1-(methoxycarbonyl)ethoxy)benzoate (7.3 g) and 60% oil dispersion (1.5 g) of sodium hydride in tetrahydrofuran (70 ml) was heated at reflux for 30 minutes, and slowly cooled to room temperature. The reaction mixture was poured into ice-aqueous ammonium chloride and extracted with ether. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was subjected to chromatography on silica gel to give 6-chloro-2-methyl-3(2H)-benzofuranone (yield, 1.8 g).

WORKUP

后处理

  1. temperatureat reflux for 30 minutes
  2. additionThe reaction mixture was poured into ice-aqueous ammonium chloride
  3. extractionextracted with ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure