HRID5803
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
A stirred mixture of 8-amino-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one hydrochloride (1.5 g) and 4H-pyran-4-one (0.84 g) in water (40 ml) was heated under reflux for 2 hours in a nitrogen atmosphere. The resultant solid was washed with dilute hydrochloric acid to give a crude product, 0.5 g. Purification by column chromatography (silica gel, 9:1 chloroform: methanol) gave the title compound 0.18 g, m.p. >300° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 2 hours in a nitrogen atmosphere
- washThe resultant solid was washed with dilute hydrochloric acid
- customto give a crude product, 0.5 g
- customPurification by column chromatography (silica gel, 9:1 chloroform: methanol)