HRID622233

反应详情

EQUATION

反应方程式

HRID 622233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 9.75 g. of ethyl 6-(4-benzylphenyl)-6-bromo-hexanoate, 5.03 g. of 2,4-dihydroxy-3-propylacetophenone, 3.57 g. of potassium carbonate, and 1.0 g. of potassium iodide in 175 ml. of acetone was heated to reflux for about 86 hours. The reaction was evaporated in vacuo and the residue was purified by chromatography over silica gel eluting with a 0-20% ethyl acetate gradient in hexane. The appropriate fractions were pooled and evaporated, giving 2.5 g. of the desired product which was used for the subsequent hydrolysis. NMR was consistent with the compound ethyl 6-(4-acetyl-3-hydroxy-2-propylphenoxy)-6-(4-benzylphenyl)hexanoate.

WORKUP

后处理

  1. temperatureto reflux for about 86 hours
  2. customThe reaction was evaporated in vacuo
  3. customthe residue was purified by chromatography over silica gel eluting with a 0-20% ethyl acetate gradient in hexane
  4. customevaporated
  5. customgiving 2.5 g