반응 #50491

반응 방정식

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

수율 23.6%

용매

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타synthesized by the method of Example 3
3. 3
   온도After cooling the reaction mixture
4. 4
   여과the precipitated crystals were collected by filtration
5. 5
   세척washed with water and ether
6. 6
   기타purified by silica gel chromatography

실험 절차

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).

출처