HRID1105686
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
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
- temperaturerefluxed under nitrogen for 24 hours
- temperatureIt is cooled to 20°
- filtrationthe solids filtered off
- washwashed with isoamyl alcohol and diethyl ether
- customrecrystallized from the mixture of 160 ml of methanol and 110 ml of water