تفاعل #9303

معادلة التفاعل

tert-butyl N-[7-iodo-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]carbamate

4,6-dimethyl-2-methoxyphenylboric acid

barium hydroxide octahydrate

ethyl acetate

→

title compound

المردود 102.9%

tert-Butyl N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]carbamate

المردود 102.9%

المذيبات

1,2-dimethoxyethane

water

Water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere added
2. 2
   درجة الحرارةthe mixture was heated
3. 3
   غسيلthe extract was washed with brine
4. 4
   تجفيفAfter drying over anhydrous magnesium sulfate and filtration
5. 5
   تركيزthe solvent was concentrated under reduced pressure
6. 6
   أخرىthe residue was purified by silica gel column chromatography

الإجراء التجريبي

After dissolving tert-butyl N-[7-iodo-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]carbamate (2.0 g) in 1,2-dimethoxyethane (60 mL) and water (30 mL), 4,6-dimethyl-2-methoxyphenylboric acid (1.33 g), tetrakis(triphenylphosphine)palladium (0) complex (865 mg) and barium hydroxide octahydrate (2.34 g) were added and the mixture was heated and stirred at 80° C. for 3 hours. Water was added to the reaction mixture, extraction was performed with ethyl acetate and the extract 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 (2.1 g) was obtained from the n-hexane:ethyl acetate (20:1) fraction as yellow amorphous.

المصدر