反应详情

温度

65 °C

In 200 ml of dimethylformamide were suspended 20 g of 3-(4-fluorophenyl)-1-(3-hydroxyphenyl)-1H-pyrazolo[3,4-b]pyridine, 21.9 g of bromoacetate and 18.1 g of potassium carbonate. The mixture was stirred at 65° C. for 4 hours. The reaction mixture was concentrated under reduced pressure. The residue was extracted with ethyl acetate-water. The organic layer was concentrated. Hexane was added to the residue for crystallization. The obtained crude crystals were recrystallized from isopropyl ether to give 10.9 g of ethyl 3-[3-(4-fluorophenyl)-1H-pyrazolo[3,4-b]pyridin-1-yl]phenoxyacetate, m.p. 130°-131° C.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionThe residue was extracted with ethyl acetate-water
3. concentrationThe organic layer was concentrated
4. additionHexane was added to the residue for crystallization
5. customThe obtained crude crystals
6. customwere recrystallized from isopropyl ether