HRID1395748
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
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
- temperaturethe mixture was refluxed for 4 hours
- temperatureAfter cooling
- filtrationthe mixture was filtered
- extractionthe filtrate was extracted with benezene
- 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