反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionThe separated aqueous phase was back-extracted twice with 100 ml of diethyl ether each time
- washThe combined organic phases were washed with 50 ml of 2N sodium carbonate solution and several times with water
- dry with materialdried over magnesium sulphate
- concentrationconcentrated
- customRecrystallization of the crude product
- customobtained from ethanol