HRID1603869

反应详情

EQUATION

反应方程式

HRID 1603869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of ethyl 4-oxo-4H-1-benzopyran-2-carboxylate (2.0 g, 9.17 mmol) in methanol (60 ml), chloroform (25 ml) and glacial acetic acid (20 ml) was added with 10% palladium-on-charcoal and the mixture was left under stirring at room pressure and temperature for 24 h. under hydrogen atmosphere. After that, the catalyst was filtered off and the filtrate was evaporated to dryness. The residue was redissolved in ethyl ether and washed successively with a 5% sodium bicarbonate solution and a sodium chloride saturated solution. The mixture was dried and the solvent was evaporated off under reduced pressure, to obtain 1.575 g of the title product (84% yield).

WORKUP

后处理

  1. waitthe mixture was left
  2. filtrationAfter that, the catalyst was filtered off
  3. customthe filtrate was evaporated to dryness
  4. dissolutionThe residue was redissolved in ethyl ether
  5. washwashed successively with a 5% sodium bicarbonate solution
  6. customThe mixture was dried
  7. customthe solvent was evaporated off under reduced pressure