HRID1926729

反应详情

EQUATION

反应方程式

HRID 1926729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-chloro-3-aminopyridazine x34 (3.16 g, 1 eq, 24.2 mmol) and 3-bromo-1,1,1-trifluorobutan-2-one (5 g, 1 eq, 24.4 mmol) in 1,2-dimethoxyethane (100 ml) is refluxed during 17 hours. After cooling to room temperature and filtration, the solvent is removed under reduced pressure and the crude mixture is purified by preparative chromatography on silicagel (CH2Cl2/MeOH/NH4OH: 98/2/0.2 (v/v/v)) leading to 6-chloro-3-methyl-2-(trifluoromethyl)imidazo[1,2-b]pyridazine x35.

WORKUP

后处理

  1. filtrationfiltration
  2. customthe solvent is removed under reduced pressure
  3. customthe crude mixture is purified by preparative chromatography on silicagel (CH2Cl2/MeOH/NH4OH: 98/2/0.2 (v/v/v))