反应详情

To a mixture of 1-(4-(7-(2-fluoro-4-nitrophenoxy)thieno[3,2-b]pyridin-2-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone (269) (358.2 mg, 0.87 mmol) and NH4Cl (39.4 mg, 0.74 mmol) in EtOH (8.7 mL)/water (4.3 mL) at 100° C. was added Fe (411.3 mg, 7.36 mmol) in one portion and the mixture heated to reflux with vigorous stirring for 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 dissolved in DCM, extracted with water, dried aver anhydrous Na2SO4 and concentrated under reduced pressure affording 270 (256.5 mg, 0.67 mmol, 77% yield) as a white solid. MS (m/z): (M+1) 384.2 (100%).

1. temperaturethe mixture 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. dissolutionThe residue was dissolved in DCM
7. extractionextracted with water
8. dry with materialdried aver anhydrous Na2SO4
9. concentrationconcentrated under reduced pressure