反应详情

温度

50 °C

To a solution of 3-hydrazino-2,5-dimethylpyrazine (2.00 g, 14.5 mmol) from Step A in 75 mL of water was added approximately 1 g (wet) Raney Ni, 50% slurry in water. After stirring at reflux for 2 h, the reaction mixture was filtered hot through Celite, and subsequently washed with hot water, followed by dichloromethane. The concentrated residues were suspended in ethylenediamine and heated at 50° C. for 30 min with stirring. Concentration followed by purification by flash chromatography (silica gel, 50% ethyl acetate/hexane) yielded the title compound. LC/MS 124 (M+1).

1. temperatureat reflux for 2 h
2. filtrationthe reaction mixture was filtered hot through Celite
3. washsubsequently washed with hot water
4. stirringwith stirring
5. concentrationConcentration
6. customfollowed by purification by flash chromatography (silica gel, 50% ethyl acetate/hexane)