HRID1181154

反应详情

EQUATION

反应方程式

HRID 1181154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-propyl-3,5-dibromo-4-nitropyrazole (19.4 g, 62 mmol), EtOH (500 ml) and benzylamine (40 g, 373 mmol) was refluxed for 15 hours. The reaction medium was concentrated to the maximum under reduced pressure. The residue was suspended in EtOAc (100 ml ), the insoluble part was separated out by filtration and the filtrate was evaporated to dryness. The black oil obtained was purified by column chromatography (eluent: EtOAc/hexane) to give the benzyl(5-bromo-4-nitro-2-propyl-2H-pyrazol-3-yl)amine in the form of a yellow solid (9 g; 29%) from 3,5-dibromo-4-nitropyrazole.

WORKUP

后处理

  1. temperaturewas refluxed for 15 hours
  2. concentrationThe reaction medium was concentrated to the maximum under reduced pressure
  3. customthe insoluble part was separated out by filtration
  4. customthe filtrate was evaporated to dryness
  5. customThe black oil obtained
  6. customwas purified by column chromatography (eluent: EtOAc/hexane)