反应详情

温度

130 °C

A suspension of 6-chloro-2-dimethylamino-1H-imidazo[4,5-c]pyridine-4-carbonitrile (100 mg, 0.45 mmol), 4-ethoxy-3-trifluoromethyl-phenyl boronic acid (198 mg, 0.88 mmol) tetrakis(triphenylphosphine)palladium(0) (50 mg, ˜10 mol %) and potassium carbonate (193.0 mg, 1.39 mmol) in THF (3 ml) was heated to 130° C. for 6 minutes in the “Smith” microwave. The crude mixture was concentrated under reduced pressure to remove THF before partitioning between ethyl acetate and water. The organic layer was separated, dried over sodium sulfate and concentrated under reduced pressure. The material was then dissolved in DMSO and purified in aliquots by preparative HPLC. The desired fractions were collected and concentrated to give a white solid which was washed with ether to afford 2-dimethylamino-6-(4-ethoxy-3-trifluoromethyl-phenyl)-1H-imidazo[4,5-c]pyridine-4-carbonitrile (5.0 mg)

1. concentrationThe crude mixture was concentrated under reduced pressure
2. customto remove THF
3. custombefore partitioning between ethyl acetate and water
4. customThe organic layer was separated
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under reduced pressure
7. dissolutionThe material was then dissolved in DMSO
8. custompurified in aliquots by preparative HPLC
9. customThe desired fractions were collected
10. concentrationconcentrated
11. customto give a white solid which
12. washwas washed with ether