HRID268036

反应详情

EQUATION

反应方程式

HRID 268036 的结构方程式

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

  1. concentrationThe reaction mixture is completely concentrated by evaporation at reduced pressure
  2. washthe organic phase is washed with a 10% sodium bicarbonate solution and with water
  3. dry with materialAfter drying over sodium sulphate
  4. concentrationconcentrating
  5. custom6,11-dihydro-11-oxo-dibenzo[b,e]thiepine-2-acetic acid ethyl ester crystallizes by the addition of ether