反応 #9278

反応方程式

7-bromo-2-ethylpyrazolo[1,5-a]pyridine

2,4-dichlorophenylboric acid

sodium carbonate

Water

→

title compound

収率 97.9%

7-(2,4-Dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridine

収率 97.9%

溶媒

ethanol

toluene

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   温度the mixture was heated
3. 3
   洗浄the organic layer was washed with brine
4. 4
   乾燥After drying over anhydrous magnesium sulfate and filtration
5. 5
   濃縮the solvent was concentrated under reduced pressure
6. 6
   その他the residue was purified by silica gel column chromatography

実験手順

After dissolving 7-bromo-2-ethylpyrazolo[1,5-a]pyridine (300 mg) in ethanol (2 mL) and toluene (4 mL), 2,4-dichlorophenylboric acid (508 mg), tetrakis(triphenylphosphine)palladium (0) complex (154 mg) and 2 M aqueous sodium carbonate (1.33 mL) were added and the mixture was heated and stirred at 80° C. for 3 hours under a nitrogen stream. Water was added to the reaction mixture, extraction was performed with ethyl acetate and the organic layer was washed with brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (380 mg) was obtained from the n-hexane:ethyl acetate (100:1) fraction as a light yellow oil.

出典