HRID1057704

反应详情

EQUATION

反应方程式

HRID 1057704 的结构方程式

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 0.5 g (1.5436 mmol) 1-chloro-4-(4-chloroanilino)phthalazine hydrochloride (for preparation see J. Chem. Soc. 1948, 777-782) and 2 g (18.50 mmol) 4-aminomethylpyridine is stirred for 36 h at 90° C. and then purified by means of flash chromatography on silica gel with a particle size of 0.04-0.06 mm using acetate and acetate/methanol (20:1). Evaporation of product-containing fractions, recrystallization of the residue from methanol, and drying of the crystallizate under HV yield the title compound; m.p. 233-236° C.; ESI-MS: (M+H)+=362.

WORKUP

后处理

  1. custompurified by means of flash chromatography on silica gel with a particle size of 0.04-0.06 mm
  2. customEvaporation of product-containing fractions, recrystallization of the residue from methanol
  3. customdrying of the crystallizate under HV