HRID476574

反应详情

EQUATION

反应方程式

HRID 476574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

23.7 g of double-distilled thionyl chloride are added dropwise to a solution, stirred and heated to 70° C., of 30.2 g of 2-(5-chloro-2,3-dihydro-2-oxo-3-phenyl-3-benzofuranyl)acetic acid in 250 ml of anhydrous benzene. When the addition is complete, the mixture is heated to reflux until the evolution of gas has completely ceased. The medium is concentrated under vacuum, the residue washed with 200 ml of anhydrous benzene and the solvent evaporated off. This operation is repeated twice and the product is left to crystallize at room temperature. The crystals are washed with petroleum ether and filtered off, and 31 g of pure product are obtained.

WORKUP

后处理

  1. additionWhen the addition
  2. temperaturethe mixture is heated
  3. temperatureto reflux until the evolution of gas
  4. concentrationThe medium is concentrated under vacuum
  5. washthe residue washed with 200 ml of anhydrous benzene
  6. customthe solvent evaporated off
  7. waitthe product is left
  8. customto crystallize at room temperature
  9. washThe crystals are washed with petroleum ether
  10. filtrationfiltered off