HRID445621

反应详情

EQUATION

反应方程式

HRID 445621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-bromo-2-chloro-3-nitropyridine (Matrix, Columbia, USA, 9.8 g, 41.3 mmol) in 250 ml THF was added 8 M methylamine in EtOH (Aldrich, Buchs, Switzerland, 12.9 ml, 103 mmol). The reaction mixture was stirred 1 h at rt then was quenched with 300 ml water. The precipite was filtered and the filtrate concentrated before being filtered again. The yellow solids were combined and dried to give the title compound as a yellow solid (HPLC: tR 3.13 min (Method A)).

WORKUP

后处理

  1. customthen was quenched with 300 ml water
  2. filtrationThe precipite was filtered
  3. concentrationthe filtrate concentrated
  4. filtrationbefore being filtered again
  5. customdried