反应详情

To a solution of 5-chloro-7-azaindole (0.50 g, 3.3 mmol) in acetic acid (5.0 mL), hexamethylenetetramine (0.69 g, 4.9 mmol) was added at ambient temperature. The mixture was refluxed for 8 h. Cooled to ambient temperature, the reaction mixture was diluted with water, extracted with ethyl acetate for 2 times. The organic layer was washed with water and brine, dried over sodium sulfate and concentrated. The residue was purified by chromatography on silica gel(hexane/ethyl acetate) to afford 5-chloro-7-azaindole-3-carboxaldehyde as solid (0.13 g, y. 22%).

1. temperatureThe mixture was refluxed for 8 h
2. extractionextracted with ethyl acetate for 2 times
3. washThe organic layer was washed with water and brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customThe residue was purified by chromatography on silica gel(hexane/ethyl acetate)