反应详情

温度

60 °C

In 75 ml of dimethylformamide were suspended 5.0 g of 3-(4-fluorophenyl)-1-(3-hydroxyphenyl)-1H-pyrazolo[3,4-b]pyridine, 3.5 g of N,N-diethylbromoacetamide and 2.5 g of potassium carbonate. The mixture was stirred at 60° C. for 5 hours. After the solvent was distilled off under reduced pressure, the residue was extracted with ethyl acetate-water. The organic layer was concentrated. Isopropyl ether was added to the residue for crystallization. The obtained crude crystals were recrystallized from ethyl acetate to give 2.8 g of N,N-diethyl-3-[3-(4-fluorophenyl)-1H-pyrazolo[3,4-b]pyridin-1yl]phenoxyacetamide, m.p. 102°-105° C.

1. distillationAfter the solvent was distilled off under reduced pressure
2. extractionthe residue was extracted with ethyl acetate-water
3. concentrationThe organic layer was concentrated
4. additionIsopropyl ether was added to the residue for crystallization
5. customThe obtained crude crystals
6. customwere recrystallized from ethyl acetate