反应详情

温度

80 °C

A mixture of 2-methoxyaniline (0.18 g), 6-chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridine (0.50 g), Cs2CO3 (0.94 g), and (2-dicyclohexylphosphino-2′,4′,6′-triisopropyl-1,1′-biphenyl)[2-(2-aminoethyl)phenyl]palladium(II) chloride (0.071 g) in toluene (6 mL) was degassed and back filled with nitrogen (3 times) before it was heated at 80° C. for overnight. The reaction was cooled and diluted with ethyl acetate (15 mL) and water (10 mL). The mixture was filtered through celite and the filtrate was separated, the organic layer was wash with with brine (10 mL), dried (MgSO4), filtered and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with EtOAc/isohexane=25% to give 6-chloro-N-(2-methoxyphenyl)-1-trityl-1H-pyrazolo[4,3-c]pyridin-3-amine (380 mg, 77% yield) as a brown solid.

1. customwas degassed
2. additionback filled with nitrogen (3 times) before it
3. temperatureThe reaction was cooled
4. additiondiluted with ethyl acetate (15 mL) and water (10 mL)
5. filtrationThe mixture was filtered through celite
6. customthe filtrate was separated
7. washthe organic layer was wash with with brine (10 mL)
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customthe solvent was evaporated under reduced pressure
11. customThe residue was purified by column chromatography on silica gel eluting with EtOAc/isohexane=25%