반응 #50492

반응 방정식

2-methyl-5-pyrazinylmethyl chloride

hydride

2-Nitromethyleneimidazolidine

hydrogen

→

1-(2-methyl-5-pyrazinylmethyl)-2-(nitromethylene)imidazolidine

수율 23.0%

용매

water

dimethylformamide

반응 조건

후처리

1. 1
   온도After cooling to room temperature
2. 2
   추출extracted with dichloromethane
3. 3
   workup.DISTILLATIONOn distilling off dichloromethane from the organic layer under reduced pressure

실험 절차

2-Nitromethyleneimidazolidine (12.9 g) was dissolved in dry dimethylformamide (100 ml), and at room temperature 60% oily soldium hydride (4.4 g) was added. The mixture was stirred at room temperature until the generation of hydrogen ceased. Then, 2-methyl-5-pyrazinylmethyl chloride (14.3 g) was added at room temperature, and the mixture was stirred at 40° C. for 8 hours. After cooling to room temperature, the reaction mixture was added to 200 ml of water, and extracted with dichloromethane. On distilling off dichloromethane from the organic layer under reduced pressure, 1-(2-methyl-5-pyrazinylmethyl)-2-(nitromethylene)imidazolidine (5.4 g) was obtained as yellow crystals having a melting point of 163° to 166° C.

출처