反应详情

温度

90 °C

A degassed mixture of tert-butyl 4-(allyl(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-6-bromo-3-(6-fluoroquinolin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)amino)piperidine-1-carboxylate (163 mg, 0.19 mmol), Pd(OAc)2 (4.3 mg, 0.02 mmol), Bu4NBr (73.6 mg, 0.23 mmol), and K2CO3 (78.7 mg, 0.57 mmol) in DMF (6 mL) was heated at 90° C. for 3 h. After cooling to room temperature, the mixture was diluted with H2O and then extracted with ethyl acetate (×2). The combined organic layers were washed with brine and dried with Na2SO4. Evaporation and purification by column chromatography afforded tert-butyl 4-(8-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-3-(6-fluoroquinolin-3-yl)-7-methyl-5H-pyrazolo[1,5-a]pyrrolo[2,3-d]pyrimidin-5-yl)piperidine-1-carboxylate: LCMS tR=1.96 Min (5 min run, UV254nm), Mass calculated for M+775.4, observed LC/MS m/z 776.0 (M+H).

1. temperatureAfter cooling to room temperature
2. extractionextracted with ethyl acetate (×2)
3. washThe combined organic layers were washed with brine
4. dry with materialdried with Na2SO4
5. customEvaporation and purification by column chromatography