反应详情

A mixture of 7-chloro-5-methyl-1H-pyrazolo[4,3-b]pyridine (1.0 g, 0.006 mole) and isobutylamine (58 g) in water (100 ml) and ethanol (50 ml) was heated under reflux for 10 days. The reaction mixture was cooled and evaporated to dryness. The oily residue was basified to pH8-9 with 10% sodium carbonate solution. The residue was extracted with ethyl acetate (3×100 ml), dried (Na2SO4) and evaporated to dryness to give a yellow oil. This was purified by column chromatography on alumina, and eluted with chloroform/methanol to give the desired compound as a white solid (500 mg). m.p. 162°-164° C.

1. temperaturewas heated
2. temperatureunder reflux for 10 days
3. temperatureThe reaction mixture was cooled
4. customevaporated to dryness
5. extractionThe residue was extracted with ethyl acetate (3×100 ml)
6. dry with materialdried (Na2SO4)
7. customevaporated to dryness
8. customto give a yellow oil
9. customThis was purified by column chromatography on alumina
10. washeluted with chloroform/methanol