HRID967013

反应详情

EQUATION

反应方程式

HRID 967013 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 7.85 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline, 13.3 g of triethylamine, 0.4 g of dimethylaminopyridine, 11.5 g of cis-decahydroquinoxaline and 80 ml of i-amyl alcohol was stirred at reflux for 72 hours. After cooling to room temperature, the solvent was evaporated off and the residue was purified by flash chromatography, eluting with petroleum ether:ethyl acetate:methanol:28% ammonium hydroxide 8:6:2:0.2. The obtained residue obtained was transformed into the hydrochloride salt and crystallized from i-propanol/methanol 1:1 to give 14.7 g (73%) of the desired compound; m.p. 290-295° C.

WORKUP

后处理

  1. temperatureat reflux for 72 hours
  2. customthe solvent was evaporated off
  3. customthe residue was purified by flash chromatography
  4. washeluting with petroleum ether
  5. customThe obtained residue obtained
  6. customcrystallized from i-propanol/methanol 1:1