反应详情

1-(4-Fluoro-phenyl)-1H-pyrazol-3-ylamine (55 mg, 0.31 mmol) was dissolved under inert gas atmosphere in dioxane (2 ml) and trimethylaluminium (0.154 ml, 2M toluene solution) was added. After stirring for 30 min at ambient temperature, 6-methyl-3-(pyrimidin-5-ylamino)-pyridine-2-carboxylic acid ethyl ester (A-1; 20 mg, 0.08 mmol) was added and the reaction mixture was heated at reflux for 18 hours. Upon cooling to room temperature water (0.5 ml) was added and intensive stirring was continued for 5 min. Sufficient sodium sulfate for water absorption and dichloromethane were added while stirring is continued. The resulting solution was then filtered through decalite and washed with dichloromethane. The solvent was evaporated and the final product was obtained after silica gel chromatography using a heptane/ethyl acetate gradient as off-white solid (5 mg, 16%).

1. temperaturethe reaction mixture was heated
2. temperatureat reflux for 18 hours
3. additionwas added
4. stirringintensive stirring
5. waitwas continued for 5 min
6. customSufficient sodium sulfate for water absorption and dichloromethane
7. additionwere added
8. stirringwhile stirring
9. filtrationThe resulting solution was then filtered through decalite
10. washwashed with dichloromethane
11. customThe solvent was evaporated