反应详情

Potassium hexamethyldisilazide (46 mg, 0.23 mmol) was added to N-[3-(aminocarbonyl)-5-ethyl-1-(2-methoxyethyl)-1H-pyrazol-4-yl]-2-butoxy-5-iodonicotinamide (Preparation 13) (100 mg, 0.19 mmol) in degassed n-butanol (2 mL) and the solution stirred under a nitrogen atmosphere. The reaction was heated at reflux for 9 h and then cooled. The butanol was removed in vacuo and the residue partitioned between dichloromethane and 1N hydrochloric acid. The organic phase was separated and washed with brine, dried (MgSO4) and concentrated to give a white solid. Trituration with ethyl acetate gave the title compound (40 mg, 42%) as a white solid.

1. temperatureThe reaction was heated
2. temperatureat reflux for 9 h
3. temperaturecooled
4. customThe butanol was removed in vacuo
5. customthe residue partitioned between dichloromethane and 1N hydrochloric acid
6. customThe organic phase was separated
7. washwashed with brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated
10. customto give a white solid