反应详情

To a solution of 4.69 g of 3-bromo-1H-pyrazolo[4,3-c]pyridine in 72 mL of dimethylformamide was added 1.42 g of sodium hydride at room temperature and stirred for 15 minutes, and then added with 6.6 g of trityl chloride and stirred at this temperature for a day. The solution was diluted with dichloromethane, and the organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The precipitated crystals were washed with ethyl acetate, the filtrate was evaporated, and the residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10-1:3), an the resultant product was combined with the above crystals, to afford 5.28 g of the title compound as colorless crystals.

1. stirringstirred at this temperature for a day
2. washthe organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was evaporated
5. washThe precipitated crystals were washed with ethyl acetate
6. customthe filtrate was evaporated
7. customthe residue was purified
8. customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:10-1:3)