HRID1105686

反应详情

EQUATION

反应方程式

HRID 1105686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 3.75 g of 8-(3-piperidinyl)-8-azaspiro[4,5]decan-7,9-dione, 3.59 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline and 100 ml of isoamyl alcohol is stirred and refluxed under nitrogen for 24 hours. It is cooled to 20°, the solids filtered off, washed with isoamyl alcohol and diethyl ether and recrystallized from the mixture of 160 ml of methanol and 110 ml of water, to yield the 8-[1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-3-piperidinyl]-8-azaspiro[4,5]decan-7,9-dione hydrochloride melting at 311°-312° with decomposition.

WORKUP

后处理

  1. temperaturerefluxed under nitrogen for 24 hours
  2. temperatureIt is cooled to 20°
  3. filtrationthe solids filtered off
  4. washwashed with isoamyl alcohol and diethyl ether
  5. customrecrystallized from the mixture of 160 ml of methanol and 110 ml of water