反应详情

温度

80 °C

To a solution of tert-butyl N-[7-bromo-2-(methoxymethyl)pyrazolo[1,5-a]pyridin-3-yl]carbamate (300 mg) dissolved in 1,2-dimethoxyethane (10 mL) and water (5 mL) was added 2,6-dimethoxy-4-methoxymethylphenylboric acid (323 mg), tetrakis(triphenylphosphine)palladium(0) (146 mg) and barium hydroxide octahydrate (398 mg), and the reaction mixture was heated and stirred for 2 hours at 80° C. under a nitrogen stream. Water was added to the obtained reaction mixture, the reaction mixture was extracted with ethyl acetate, and the organic extract was washed with brine. The obtained organic extract was dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography and the title compound (245 mg) was obtained as a light yellow amorphous solid from the n-hexane:ethyl acetate (1:1) fraction.

1. temperaturethe reaction mixture was heated
2. extractionthe reaction mixture was extracted with ethyl acetate
3. extractionthe organic extract
4. washwas washed with brine
5. extractionThe obtained organic extract
6. dry with materialwas dried over anhydrous magnesium sulfate
7. filtrationfiltered
8. customthe solvent was evaporated under reduced pressure
9. customThe residue was purified by silica gel column chromatography