HRID29414

反应详情

EQUATION

反应方程式

HRID 29414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 4-hydroxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester 0.5 g (2.27 mmol) was added 15 mL of chlorobenzene, 0.27 g (3.4 mmol) of acetyl chloride and 0.63 mL (5.7 mmol) of titanium tetrachloride. The mixture was sealed in a pressure tube and the tube was placed in 95° C. oil bath for 5 h with stirring. The reaction mixture was washed with 0.5N HCl and was extracted with ethyl acetate. Removal of the solvents gave the crude product, which was purified by column chromatography to give 0.33 g (59% yield) of 5-acetyl-4-hydroxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester as a white solid.

WORKUP

后处理

  1. customThe mixture was sealed in a pressure tube
  2. customwas placed in 95° C.
  3. customfor 5 h
  4. washThe reaction mixture was washed with 0.5N HCl
  5. extractionwas extracted with ethyl acetate
  6. customRemoval of the solvents
  7. customgave the crude product, which
  8. customwas purified by column chromatography