HRID1395748

反应详情

EQUATION

反应方程式

HRID 1395748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 172 mg of ethyl 2-(10,11-dihydro-11-oxo dibenzo [b,f]-thiepin-3-yl)-propionate in 1 ml of toluene were added a small amount of zinc-amalgam, 0.5 ml of conc. hydrochloric acid and 0.4 ml of water and the mixture was refluxed for 4 hours. After cooling, the mixture was filtered and the filtrate was extracted with benezene. 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 subjected to thin-layer chromatography and there was obtained 26 mg of ethyl 2-(10,11-dihydro dibenzo[b,f]thiepin-3-yl)-propionate as pale yellow oil.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 4 hours
  2. temperatureAfter cooling
  3. filtrationthe mixture was filtered
  4. extractionthe filtrate was extracted with benezene
  5. washThe extract was washed with saturated sodium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off
  8. customto obtain yellow oil, which