反应详情

To a slurry of iron powder (5.32 g, 95 mmol) in MeOH/H2O/HOAc (7.5 mL/7.5 mL/0.30 mL) at 75° C. was added 5-nitro-2-[(phenylmethyl)oxy]pyridine (3.10 g, 13.4 mmol; step A above), portionwise over 20 min. After 2 h, the mixture was cooled, 1M NaOH (10 mL) was added. The mixture was filtered through Celite (MeOH wash×2) and concentrated in vacuo. The residue was purified by flash chromatography (EtOAc/hexanes), affording 2.21 g of the title compound as an orange syrup: MS (ESI) m/z 201 (M+1).

1. waitAfter 2 h
2. temperaturethe mixture was cooled
3. filtrationThe mixture was filtered through Celite (MeOH wash×2)
4. concentrationconcentrated in vacuo
5. customThe residue was purified by flash chromatography (EtOAc/hexanes)