Reaktion #464174

ord-6edf7b5b17224a0b9a1b86f19c38020d

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

2-Nitromethyleneimidazolidine (12.9 g) was dissolved in dry dimethylformamide (100 ml), and at room temperature 60% oily sodium 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06022967uspto-grants-2000_02