反应详情

To a solution of 5-bromo-1H-indole-7-carboxamide (10 g, 41.84 mmol) in methanol (5 mL), 1,1-dimethylethyl 4-oxo-1-piperidinecarboxylate (684 mg, 3.42 mmol) and sodium methoxide (0.5 M in THF, 13.7 mL, 6.84 mmol) were added. The reaction mixture was stirred at reflux temperature for 16 hours. All solvent was evaporated under reduced pressure. The residue was partitioned between ethyl acetate (100 mL) and water (100 mL). The combined organic phase was dried over MgSO4 and concentrated under reduced pressure, and purified by flash column chromatography (ethyl acetate/hexanes, 1/1) to give the desired product (7.4 g, 43%).

1. temperatureat reflux temperature for 16 hours
2. customAll solvent was evaporated under reduced pressure
3. customThe residue was partitioned between ethyl acetate (100 mL) and water (100 mL)
4. dry with materialThe combined organic phase was dried over MgSO4
5. concentrationconcentrated under reduced pressure
6. custompurified by flash column chromatography (ethyl acetate/hexanes, 1/1)