反应详情

温度

60 °C

To a solution of ethyl 2-chloro-3-cyano-6-methylisonicotinate (1.0 g, 4.5 mmol) in EtOH (14.8 mL) is added Raney nickel (100 mg, RANEY 2800 NICKEL), and the mixture is stirred at 60° C. under hydrogen atmosphere for 2 days. After cooling to rt, the reaction mixture is filtered through a pad of Celite™. The filtrate is concentrated, and the residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (1:1), and the collecting sample is recrystallized from THF/n-hexane to give 91 mg (11% yield) of the title compound as white solid.

1. temperatureAfter cooling to rt
2. filtrationthe reaction mixture is filtered through a pad of Celite™
3. concentrationThe filtrate is concentrated
4. customthe residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (1:1)
5. customthe collecting sample is recrystallized from THF/n-hexane