反应详情

温度

85 °C

Part B. The product from Part A (5.50 g, 41.98 mmol) and 2,2,2-trifluoro-N-(4-methoxyphenyl)-ethanehydrazonoyl bromide (12.90 g, 43.58 mmol) were stirred in toluene (100 mL) at room temperature under N2. Et3N (28.0 mL, 200.1 mmol) was then added. The mixture was stirred at 85° C. for 15 h. It was cooled to room temperature and extracted with EtOAc (3×). The organic layers were washed with H2O (2×) and brine (2×), dried over MgSO4, filtered, and concentrated to dryness. The residue was purified by flash column chromatography (silica gel, CH2Cl2, then CH2Cl2:EtOAc=4:1, then EtOAc) to produce 1-(4-methoxyphenyl)-3-(trifluoromethyl)-1,4,5,6-tetrahydro-7H-pyrazolo[3,4-c]pyridin-7-one as a light-tan solid (5.09 g, yield: 39%). LC/MS (ESI+) 312.4 (M+H)+.

1. temperatureIt was cooled to room temperature
2. extractionextracted with EtOAc (3×)
3. washThe organic layers were washed with H2O (2×) and brine (2×)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated to dryness
7. customThe residue was purified by flash column chromatography (silica gel, CH2Cl2