反应详情

To a mixture of 7-(2-fluoro-4-nitrophenoxy)-N′,N′-dimethylthieno[3,2-b]pyridine-2-carbohydrazide 238 (772 mg, 2.05 mmol) and NH4Cl (93 mg, 1.74 mmol) in EtOH (20.5 mL)/water (10.3 mL) at 100° C., Fe (973 mg, 17.73 mmol) was added in one portion and the mixture was heated to reflux with vigorous stirring 40 min. The mixture was filtered through Celite®, the Celite® washed with EtOH and the combined organic solutions concentrated under reduced pressure. The residue was purified by flash chromatography (MeOH/DCM 1:9) giving 239 (605 mg, 1.75 mmol, 85%). MS (m/z): (M+1) 347.0 (100%).

1. temperaturethe mixture was heated
2. temperatureto reflux
3. filtrationThe mixture was filtered through Celite®
4. washthe Celite® washed with EtOH
5. concentrationthe combined organic solutions concentrated under reduced pressure
6. customThe residue was purified by flash chromatography (MeOH/DCM 1:9)