反应详情

To 300 mg of 2-(10,11-dihydro-11-oxo dibenzo[b,f]thiepin-3-yl)-propionamide in 3 ml of ethanol was added 0.3 ml of conc. sulfuric acid and the mixture was refluxed for 3.5 hours. The solvent was distilled off to obtain the residue, to which was added pieces of ice, and the 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, and there was obtained 277 mg of ethyl 2-(10,11-dihydro-11-oxo dibenzo[b,f]thiepin-3-yl)-propionate as pale brown oil.

1. temperaturethe mixture was refluxed for 3.5 hours
2. distillationThe solvent was distilled off
3. customto obtain the residue
4. additionto which was added pieces of ice
5. extractionthe mixture was extracted with ethyl acetate
6. washThe extract was washed with saturated sodium chloride solution
7. dry with materialdried over anhydrous sodium sulfate
8. distillationThe solvent was distilled off
9. customto obtain brown oil, which
10. customwas chromatographed over silica gel
11. washeluted with chloroform