反应详情

To a solution of 2-(difluoromethoxy)-5-nitropyridine (0.900 g, 2.35 mmol) in ethanol (5.0 mL), was added iron powder (0.400 g, 7.14 mmol) and conc. HCl (0.2 mL). The reaction mass was refluxed for ½ h. Ethanol was removed under vacuum. To the reaction mass, water was added, basified with NaHCO3 and extracted with DCM. The organic layer was separated, dried over anhydrous sodium sulphate and concentrated to afford 0.400 g of the desired product. 1HNMR (DMSO-d6): δ 7.65 (s, 1H), 7.52-7.03 (t, J=72.0 Hz, 1H), 7.27 (s, 1H), 6.73 (d, J=8.4 Hz, 1H); MS [M−H]−: 159.14.

1. temperatureThe reaction mass was refluxed for ½ h
2. customEthanol was removed under vacuum
3. additionTo the reaction mass, water was added
4. extractionextracted with DCM
5. customThe organic layer was separated
6. dry with materialdried over anhydrous sodium sulphate
7. concentrationconcentrated