反应详情

A solution of 7-azaindole (20.0 g, 169 mmol) in ethanol (200 ml) was treated with wet Raney Nickel (4 g, 50% water) and stirred in a hydrogen atmosphere at 5 atmospheres pressure at 95° C. over 2 days. The reaction mixture was filtered through diatomaceous earth and the filtrate evaporated under vacuum. The residue was purified by column chromatography eluting with ethyl acetate followed by increasingly polar mixtures of methylene chloride and methanol (saturated with ammonia) to give 7-azaindoline (12.1 g, 79%).

1. filtrationThe reaction mixture was filtered through diatomaceous earth
2. customthe filtrate evaporated under vacuum
3. customThe residue was purified by column chromatography
4. washeluting with ethyl acetate
5. temperatureby increasingly polar mixtures of methylene chloride and methanol (saturated with ammonia)