反应 #50491

反应方程式

2,2,2-trifluoroethanol sodium salt

Sodium hydride

2,2,2-trifluoroethanol

1-(2-chloro-5-pyridylmethyl)-2-(nitroimino)imidazolidine

hydrogen

→

1-[2-(2,2,2-trifluoroethoxy)-5-pyridylmethyl]-2-(nitroimino)imidazolidine

收率 23.6%

溶剂

toluene

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   其他synthesized by the method of Example 3
3. 3
   温度After cooling the reaction mixture
4. 4
   过滤the precipitated crystals were collected by filtration
5. 5
   洗涤washed with water and ether
6. 6
   其他purified by silica gel chromatography

实验过程

Sodium hydride (0.48 g) was added to a solution of 2,2,2-trifluoroethanol (2.4 g) in toluene (30 ml) was added, and the mixture was stirred until the generation of hydrogen ceased. As a result, 2,2,2-trifluoroethanol sodium salt was prepared. To the product were added 1-(2-chloro-5-pyridylmethyl)-2-(nitroimino)imidazolidine (5.1 g) synthesized by the method of Example 3 and a catalytic amount of 4-dimethylaminopyridine. The mixture was heated at 80° C. for 10 hours with stirring. After cooling the reaction mixture, the precipitated crystals were collected by filtration, washed with water and ether and then purified by silica gel chromatography to give 1-[2-(2,2,2-trifluoroethoxy)-5-pyridylmethyl]-2-(nitroimino)imidazolidine (1.5 g).

来源