HRID1395755
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To 50 mg of 2-(10,11-dihydro-11-oxo dibenzo[b,f]oxepin-3-yl)-propionamide in 2 ml of ethanol was added 0.2 ml of conc. sulfuric acid and the mixture was refluxed with stirring for 5 hours. The solvent was distilled off to obtain the residue, which 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 yellow oil, which was chromatographed over silica gel, eluted with chloroform and there was obtained 55 mg of ethyl 2-(10,11-dihydro-11-oxo dibenzo[b,f]oxepin-3-yl)-propionate as pale yellow oil.
WORKUP
后处理
- temperaturethe mixture was refluxed
- distillationThe solvent was distilled off
- customto obtain the residue, which
- extractionwas 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 yellow oil, which
- customwas chromatographed over silica gel
- washeluted with chloroform