HRID973269

反应详情

EQUATION

反应方程式

HRID 973269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 12.0 parts of 6,8-di-t-butyl-4-oxo-4H-1benzopyran-2-carboxylic acid, ethyl ester in 150 parts of ethanoo was hydrogenated, using Raney Nickel as catalyst, until one equivalent of hydrogen had been absorbed. The catalyst was removed by filtration and the ethanol was evaporated to give a residue which was chromatographed on silica gel. Careful elution with a 1:1 mixture of chloroform and light petroleum (b.p. 60°-80° C) gave 3.73 parts of 6,8-di-t-butyl-2,3-dihydro-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester, m.p. 61°-63° C, as a yellow solid.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. customthe ethanol was evaporated
  3. customto give a residue which
  4. customwas chromatographed on silica gel
  5. washCareful elution
  6. additionwith a 1:1 mixture of chloroform and light petroleum (b.p. 60°-80° C)