HRID1417101

反应详情

EQUATION

反应方程式

HRID 1417101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(4-hydroxyphenyl)-2,2-dimethylpropanoic acid ethyl ester (12.2 g) was added to a slurry containing 6.46 g of potassium tert-butoxide in 55 ml dry dimethylformamide at 0° C. After 30 minutes, a solution containing 12.6 g of ethyl (α-bromo-ortho-toluate in 15 ml dry dimethylformamide was added and the solution stirred for 2 hours at room temperature, then at 50° C. overnight. Dilution with water, extraction with ether and evaporation left an oil which was purified by HPLC (silica gel, 7:3 dichloromethane-heptane) to give 20.3 g of 2-[4-(2-ethoxycarbonyl-2-methylpropyl)phenoxymethyl]benzoic acid ethyl ester as an oil.

WORKUP

后处理

  1. additionwas added
  2. customat 50° C.
  3. customovernight
  4. extractionDilution with water, extraction
  5. customwith ether and evaporation
  6. waitleft an oil which
  7. customwas purified by HPLC (silica gel, 7:3 dichloromethane-heptane)