反应详情

A suspension of 6-chloro-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridine-5-carbaldehyde (5 g, 0.023 mol) and potassium carbonate (9.9 g, 0.0717 mol) in DMF (75 mL) was stirred for 20 min at RT. Cyclopentylmethyl ethyl amine (4.25 g, 33.0 mmol) was then added and the reaction was refluxed for 8 h. After cooling the reaction to RT, water (500 mL) was added to the reaction mixture and extracted with ethyl acetate (3×400 mL) and the combined organic layers were dried and concentrated. The residue was purified by silica gel (100-200 mesh) column chromatography. Elution with 10% ethyl acetate in hexanes gave the pure product as a colorless, gummy mass (yield: 76%).

1. temperaturethe reaction was refluxed for 8 h
2. temperatureAfter cooling
3. customthe reaction to RT
4. extractionextracted with ethyl acetate (3×400 mL)
5. customthe combined organic layers were dried
6. concentrationconcentrated
7. customThe residue was purified by silica gel (100-200 mesh) column chromatography
8. washElution with 10% ethyl acetate in hexanes
9. customgave the pure product as a colorless, gummy mass (yield: 76%)