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
The mixture of 83 mg of ethyl 2-(10,11-dihydro-11-oxo dibenzo[b,f]thiepin-3-yl)-propionate, 0.8 ml of ethanol, 120 mg of potassium hydroxide and 0.8 ml of water was stirred at room temperature for 2 hours. The solvent was distilled off to obtain the residue, which was acidified with hydrochloric acid and the resulting mixture was extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain brown oil, which was chromatographed over silica gel, eluted with chloroform to give 59 mg of 2-(10,11-dihydro-11-oxo dibenzo[b,f]thiepin-3-yl)-propionic acid as pale yellow oil. The result in IR spectrum thereof is in accordance with that of the compound obtained in Example 9.
WORKUP
后处理
- distillationThe solvent was distilled off
- customto obtain the residue, which
- extractionthe resulting mixture was extracted with ethyl acetate
- washThe extract was washed with saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent was distilled off
- customto obtain brown oil, which
- customwas chromatographed over silica gel
- washeluted with chloroform