HRID329289

反应详情

EQUATION

反应方程式

HRID 329289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of ethyl 8-acetyl-12,13-epoxytridecanoate (14.9 g., 0.05 mole), 4-tert-butylphenol (11.2 g., 0.075 mole), sodium hydroxide (7.0 g., 0.175 mole), water (30 ml.) and tetrahydrofuran (200 ml.) is stirred 4 hours at 40°-45°, 17 hours at 25° and one hour on the steam bath letting the tetrahydrofuran slowly boil away. The residue is treated with water and extracted with ether. The aqueous solution is acidified with hydrochloric acid. The oily product is taken up in ether. The ether is evaporated and the residue treated with a solution of 16.8 g. sodium bicarbonate in 275 ml. of water. The resulting solution is extracted twice with ether to remove the excess weakly acidic phenol. The aqueous solution is acidified, the product taken up in ether, washed with water and dried over sodium sulfate. The ether is evaporated leaving 10.2 g. of the crude title compound as a yellow viscous oil.

WORKUP

后处理

  1. extractionextracted with ether
  2. customThe ether is evaporated
  3. additionthe residue treated with a solution of 16.8 g
  4. extractionThe resulting solution is extracted twice with ether
  5. customto remove the excess weakly acidic phenol
  6. washwashed with water
  7. dry with materialdried over sodium sulfate
  8. customThe ether is evaporated
  9. customleaving 10.2 g