反应详情

温度

85 °C

3-Bromo-6-(difluoromethoxy)pyrazolo[1,5-a]pyrimidine (0.030 g, 0.114 mmol), tert-butyl[(1R,2R)-2-({[5-ethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)thiophen-2-yl]carbonyl}amino)-3,3-difluorocyclohexyl]carbamate (0.059 g, 0.115 mmol), Pd(PPh3)4 (6.57 mg, 0.007 mmol), and 2 M Na2CO3 (aq) (0.170 mL, 0.341 mmol) were placed in a sealed tube and DMF (1.14 mL) added. The mixture was purged with N2 for 5 min. The reaction was heated to 85° C. for 16 h. The mixture was cooled to room temperature, diluted with dichloromethane, and washed twice with saturated sodium bicarbonate (aq) and once with brine. The organic layer was dried with sodium sulfate, filtered, and concentrated under reduced pressure. The crude product was purified by column chromatography (0-70% EtOAc/Hex) to give the title compound (0.037 g, 0.064 mmol). LRMS (APCI) calc'd for (C25H29F4N5O4S) [M+H]+, 572.2; found 572.1.

1. customThe mixture was purged with N2 for 5 min
2. temperatureThe mixture was cooled to room temperature
3. additiondiluted with dichloromethane
4. washwashed twice with saturated sodium bicarbonate (aq) and once with brine
5. dry with materialThe organic layer was dried with sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe crude product was purified by column chromatography (0-70% EtOAc/Hex)