HRID2050419

反应详情

EQUATION

反应方程式

HRID 2050419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 17 g of methyl 4-(9-decenyloxy)benzoate. 17 g of potassium hydroxide, 20 ml of water and 200 ml of methanol was heated to 75° C. on an oil bath for 4 hours. The cooled mixture was treated with 100 ml of ice-cold 3N hydrochloric acid and the liberated acid was taken up in 150 ml of diethyl ether. The separated aqueous phase was back-extracted twice with 100 ml of diethyl ether each time. The combined organic phases were washed with 50 ml of 2N sodium carbonate solution and several times with water, dried over magnesium sulphate and concentrated. Recrystallization of the crude product obtained from ethanol gave 7 g of 4-(9-decenyloxy)benzoic acid, m.p. (C-SC) 77° C., phase transition (SC -N) 116° C., cl.p. (N-I) 137° C.

WORKUP

后处理

  1. extractionThe separated aqueous phase was back-extracted twice with 100 ml of diethyl ether each time
  2. washThe combined organic phases were washed with 50 ml of 2N sodium carbonate solution and several times with water
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated
  5. customRecrystallization of the crude product
  6. customobtained from ethanol