HRID261448

反应详情

EQUATION

反应方程式

HRID 261448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A 4.2 g sample of 6-carbomethoxy-7,8-dihydroxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine is slurried in 25 ml of acetone and 0.7 g (0.016 mol, 10% excess) of ethylene oxide is added. The mixture is placed in a pressure bottle and stirred at ambient temperature for about 40 hours. The reaction mixture is then heated to 60°-80° for 30 minutes, cooled and filtered. Concentration of the filtrate gives a solid which is taken up in ethyl acetate and reprecipitated with ether. The solid thus obtained is dissolved in ethanol and treated with ethereal hydrogen chloride to give 6-carbomethoxy-7,8-dihydroxy-3-(2-hydroxyethyl)-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride.

WORKUP

后处理

  1. temperatureThe reaction mixture is then heated to 60°-80° for 30 minutes
  2. temperaturecooled
  3. filtrationfiltered
  4. customConcentration of the filtrate gives a solid which
  5. customreprecipitated with ether
  6. customThe solid thus obtained