HRID375611

反应详情

EQUATION

反应方程式

HRID 375611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1 g of 1,3-dichloro-7,8,9,10-tetrahydroazepino[2,1-b]quinazolin-12(6H)-one in 15 mL of triethylsilane was added 8 g of anhydrous zinc chloride and the mixture was refluxed under nitrogen with vigorous stirring. The triethylsilane was replenished in about 8-hour intervals. When the reaction was judged complete by TLC (300:25:1 chloroform:methanol: 28% aqueous ammonia, basified aliquot) the excess of triethylsilane and other volatiles were removed in vacuo and the residue was purified and worked-up as in Method A to give the desired 1,3-dichloro-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazoline hydrochloride as white crystalline solid.

WORKUP

后处理

  1. temperaturethe mixture was refluxed under nitrogen with vigorous stirring
  2. customwere removed in vacuo
  3. customthe residue was purified and worked-up as in Method A