HRID268036
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
40 g of 6,11-dihydro-11-oxo-dibenzo[b,e]thiepine-2-acetic acid are boiled at reflux for 45 minutes together with 400 cc of 3 N hydrochloric acid in ethanol. The reaction mixture is completely concentrated by evaporation at reduced pressure and the oily residue is divided between ethyl acetate and water; the organic phase is washed with a 10% sodium bicarbonate solution and with water. After drying over sodium sulphate and concentrating, 6,11-dihydro-11-oxo-dibenzo[b,e]thiepine-2-acetic acid ethyl ester crystallizes by the addition of ether. (M.P. 98°-100°).
WORKUP
后处理
- concentrationThe reaction mixture is completely concentrated by evaporation at reduced pressure
- washthe organic phase is washed with a 10% sodium bicarbonate solution and with water
- dry with materialAfter drying over sodium sulphate
- concentrationconcentrating
- custom6,11-dihydro-11-oxo-dibenzo[b,e]thiepine-2-acetic acid ethyl ester crystallizes by the addition of ether