HRID445919

反应详情

EQUATION

反应方程式

HRID 445919 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-chloro-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-6-amine (1.05 g, 3.95 mmol), (4-aminophenyl)(morpholino)methanone (1.630 g, 7.90 mmol), and N,N-diisopropylethylamine (1.243 mL, 7.11 mmol) in 1,4-dioxane (60 mL) was heated at reflux for 2 days. The volatiles were removed under vacuum. To the residue was added water (60 mL). The precipitating material was collected by suction filtration. The filter cake was purified by ISCO (120 g silica gel, solid loading, 3-8% MeOH/CH2Cl2) to provide the desired product, (4-(6-amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5-ylamino)phenyl)(morpholino)methanone (0.595 g, 1.339 mmol, 33.9% yield), as a yellow solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 days
  3. customThe volatiles were removed under vacuum
  4. additionTo the residue was added water (60 mL)
  5. filtrationThe precipitating material was collected by suction filtration
  6. customThe filter cake was purified by ISCO (120 g silica gel, solid loading, 3-8% MeOH/CH2Cl2)