反应详情

温度

120 °C

A mixture of 2-methoxymethyl-4-tributylstannanyl-pyridine 8AN (0.1 g, 0.24 mmol), 3-bromo-5-nitro-1-trityl-1H-indazole 1AJ (0.12 g, 0.24 mmol), CsF (0.08 g, 0.53 mmol), [Pd2(dba)3] (5 mg, 0.005 mmol), Pd[P(t-Bu)3)2, and CuI (4 mg, 0.024 mmol) in DMF (2 ml) was degassed for 5 minutes. Then it was heated at 120° C. for two hours. Cooled to room temperature and diluted with EtOAc (10 ml). It was then filtered on a celite pad. Filtrate was washed with water (3 ml) and the organic extracts were dried over MgSO4. It was filtered again on a celite pad and concentrated. The residue was purified on silica gel eluting with 2/1 EtOAc/Hexane to give the desired product 3-(2-methoxymethyl-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole 9AN (0.095 g, 76%).

1. customwas degassed for 5 minutes
2. temperatureCooled to room temperature
3. additiondiluted with EtOAc (10 ml)
4. filtrationIt was then filtered on a celite pad
5. washFiltrate was washed with water (3 ml)
6. dry with materialthe organic extracts were dried over MgSO4
7. filtrationIt was filtered again on a celite pad
8. concentrationconcentrated
9. customThe residue was purified on silica gel eluting with 2/1 EtOAc/Hexane