HRID562574

反应详情

EQUATION

反应方程式

HRID 562574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 143.0 g (0.46 mol) of N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidine-amine in 7.15 liters of ethyl acetate is stirred with 14.3 g of palladium on active carbon (10% Pd) under a hydrogen atmosphere at normal pressure for 6.5 hours. The suspension is filtered and the filtrate is concentrated in a rotary evaporator. The crude product is recrystallised from methylene chloride, yielding N-(5-amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidine-amine; m.p. 138° C.-140° C., Rf=0.36 (methylene chloride:methanol=9:1).

WORKUP

后处理

  1. filtrationThe suspension is filtered
  2. concentrationthe filtrate is concentrated in a rotary evaporator
  3. customThe crude product is recrystallised from methylene chloride