反应详情

温度

80 °C

To a solution of 7-bromo-2-ethyl-3-nitropyrazolo[1,5-a]pyridine (1.0 g) dissolved in a mixture of 1,2-dimethoxyethane (50 mL) and water (25 mL) was added 2,6-dimethoxy-4-(methoxymethyl)phenylboric acid (1.26 g), tetrakis(triphenylphosphine)palladium(0) (0.64 g) and barium hydroxide octahydrate (1.75 g), and the reaction mixture was heated and stirred for 2 hours at 80° C. To the resultant reaction mixture was added water and ethyl acetate, and remove insoluble residue was filtered out with celite. The filtrate was extracted with ethyl acetate, the organic extract was washed with brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography and the title compound (0.77 g) was obtained as yellow crystals from the n-hexane:ethyl acetate (3:1) fraction.

1. temperaturethe reaction mixture was heated
2. customTo the resultant reaction mixture
3. customremove insoluble residue
4. filtrationwas filtered out with celite
5. extractionThe filtrate was extracted with ethyl acetate
6. extractionthe organic extract
7. washwas washed with brine
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationfiltered
10. customthe solvent was evaporated under reduced pressure
11. customThe obtained residue was purified by silica gel column chromatography