反应详情

11 g (40 mmol) (6-benzyloxy-3-nitro-pyridin-2-yl)-acetonitrile and 1.7 g Raney nickel (washed with abs. EtOH) in 120 mL EtOH and 50 mL acetic acid were hydrogenated at RT in a hydrogen atmosphere of 3 bar. The catalyst was filtered off and the filtrate was evaporated down. The residue was combined with 30 mL water and adjusted to pH=10 with solid sodium carbonate. The aqueous phase was extracted several times with EtOAc. The combined organic phases were dried on magnesium sulphate, filtered and evaporated down. The residue was purified by flash chromatography. The product-containing fractions were combined and evaporated down.

1. filtrationThe catalyst was filtered off
2. customthe filtrate was evaporated down
3. extractionThe aqueous phase was extracted several times with EtOAc
4. customThe combined organic phases were dried on magnesium sulphate
5. filtrationfiltered
6. customevaporated down
7. customThe residue was purified by flash chromatography
8. customevaporated down