HRID431402

反应详情

EQUATION

反应方程式

HRID 431402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

0.88 g of 5-chloro-1,3-dimethyl-4-nitro-1H-pyrazole (Aldrich), 1 molar equivalent of triethylamine, 1.1 molar equivalents of 3-imidazol-1-ylpropylamine and 5 ml of N,N-dimethylformamide were introduced into a 25 ml three-necked round-bottomed flask equipped with a magnetic stirrer, a thermometer and a condenser. The reaction medium was maintained at a temperature of about 105° C. for 6 hours. The solvent was evaporated off under vacuum. A black liquid was obtained, which was purified by chromatography on silica gel (ethyl acetate/methanol=4/1). 0.75 g of (2,5-dimethyl-4-nitro-2H-pyrazol-3-yl)(3-imidazol-1-yl-propyl)amine was obtained in the form of white crystals in a yield of 56.7%.

WORKUP

后处理

  1. customequipped with a magnetic stirrer
  2. customThe solvent was evaporated off under vacuum
  3. customA black liquid was obtained
  4. customwhich was purified by chromatography on silica gel (ethyl acetate/methanol=4/1)