反应详情

温度

50 °C

A mixture of 1-chloro-4,5-difluoro-2-nitrobenzene (2.23 g, 11.5 mmol), 1-(4-methoxybenzyl)-3-iodo-1H-pyrazolo[3,4-b]pyridin-4-ol (4.00 g, 10.5 mmol), K2CO3 (1.60 g, 11.5 mmol) and DMF (100 mL) was heated to 50° C. for 18 hours. The reaction was cooled to ambient temperature, diluted with water (500 mL), extracted with EtOAc, dry over sodium sulfate, filter and concentrate. The residue was purified by flash column chromatography (5% MeOH in CH2Cl2) to provide a light pink solid. The solid was triturated with hot MeOH to afford the product (2.35 g, 40% yield) as a white solid. LRMS (APCI pos) m/e 554.8 (M+H).

1. temperatureThe reaction was cooled to ambient temperature
2. extractionextracted with EtOAc
3. dry with materialdry over sodium sulfate
4. filtrationfilter
5. concentrationconcentrate
6. customThe residue was purified by flash column chromatography (5% MeOH in CH2Cl2)
7. customto provide a light pink solid
8. customThe solid was triturated with hot MeOH