反应详情

温度

60 °C

To (5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)-(2-fluoro-3-nitro-phenyl)-methanone (18, 2.27 g, 6.23 mmol) in 200 mL of tetrahydrofuran and 200 mL of ethyl acetate, stannous chloride, dehydrate (4.85 g, 2.15 mmol) is added. The reaction is heated at 60° C. for 3 days, then 300 mL of water and 200 mL of ethyl acetate are added. The mixture is treated with celite and filtered. Brine is added, the organic layer is separated, dried over magnesium sulfate, filtered and the filtrate is concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with ethyl acetate and hexane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound (19, 972 mg).

1. additionThe mixture is treated with celite and
2. filtrationfiltered
3. additionBrine is added
4. customthe organic layer is separated
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationthe filtrate is concentrated under vacuum
8. customThe resulting material is purified by silica gel column chromatography
9. washeluting with ethyl acetate and hexane
10. concentrationconcentrated under vacuum