反応 #50491

反応方程式

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

収率 23.6%

溶媒

toluene

反応条件

後処理

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

実験手順

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).

出典