HRID42002

反应详情

EQUATION

反应方程式

HRID 42002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 6-chloropyridin-3-amine (11.67 mmol, 1.5 g) and 2-bromo-5-methylbenzoic acid (23.34 mmol, 5.02 g), Cu (1.17 mmol, 0.1 g), Cu2O (0.58 mmol, 0.1 g) and K2CO3 (23.34 mmol, 3.2 g) in 1,2-dimethoxyethane (15 ml) was heated at 130° C. for 16 hours, under argon atmosphere. Water was added and the mixture was filtered through celite. HCl 2N aqueous solution was added until pH 6 and the solid formed was filtered off. The crude was purified by chromatography eluting with DCM/MeOH mixtures affording 1.40 g (yield 46%).

WORKUP

后处理

  1. filtrationthe mixture was filtered through celite
  2. additionHCl 2N aqueous solution was added until pH 6
  3. customthe solid formed
  4. filtrationwas filtered off
  5. customThe crude was purified by chromatography
  6. washeluting with DCM/MeOH
  7. custommixtures affording 1.40 g (yield 46%)