反应详情

To a mixture of 4-(7-(2-fluoro-4-nitrophenoxy)thieno[3,2-b]pyridin-2-yl)-1-methyl-1,2,3,6-tetrahydropyridine 259 (279 mg, 0.72 mmol) and NH4Cl (33 mg, 0.612 mmol) in EtOH (7.2 mL)/water (3.6 mL) at 100° C. Fe (342 mg, 6.2 mmol) was added 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 MeOH and purified by flash chromatography (DCM/MeOH 5:1) giving 260 (171.3 mg, 0.48 mmol, 67% yield) as a yellow solid. MS (m/z): (M+1) 356.0 (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 MeOH
7. custompurified by flash chromatography (DCM/MeOH 5:1)