HRID2177016

反应详情

EQUATION

反应方程式

HRID 2177016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

(Ref: J. Org. Chem. 1955; 20; 813-818) A solution of 2-chloro-1-(5-chloro-2-hydroxy-phenyl)-ethanone (5 g; 24.4 mmol) in ethanol was heated to reflux for 10 minutes and sodium acetate (2 g; 24.4 mmol) was added to the hot mixture. Mixture continued to reflux an additional 10 minutes, and reaction was stoppered and chilled to 0° C. for 20 minutes. Mixture was quenched with water and mixture extracted with ethyl acetate (3×75 mL). Combined organics was washed with brine and dried over MgSO4. Crude material was purified by chromatography using 0-1% methanol/DCM to afford 5-chlorobenzofuran-3-one as a oily solid. (3.0 g; 75% yield).

WORKUP

后处理

  1. temperatureto reflux for 10 minutes
  2. temperatureto reflux an additional 10 minutes
  3. customreaction
  4. customMixture was quenched with water and mixture
  5. extractionextracted with ethyl acetate (3×75 mL)
  6. washCombined organics was washed with brine
  7. dry with materialdried over MgSO4
  8. customCrude material was purified by chromatography