HRID1164808

反应详情

EQUATION

反应方程式

HRID 1164808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours in a nitrogen atmosphere
  3. washThe resultant solid was washed with dilute hydrochloric acid
  4. customto give a crude product, 0.5 g
  5. customPurification by column chromatography (silica gel, 9:1 chloroform:methanol)