反应详情

温度

100 °C

6-chloro-N-methyl-1-trityl-1H-pyrazolo[4,3-c]pyridin-3-amine (400 mg, 0.941 mmol), 1-(phenyl(tetrahydrofuran-2-yl)methyl)urea (228 mg, 1.035 mmol), cesium carbonate (920 mg, 2.82 mmol) and BrettPhos precatalyst (52.6 mg, 0.066 mmol) were taken up in dioxane (9.5 ml) in a 20 mL microwave vial. The vial was evacuated and back-filled with N2 (×3). The reaction mixture was stirred at 100° C. for two hours. Room temperature was attained. The crude reaction mixture was diluted with EtOAc and filtered through celite. The filtrate was concentrated in vacuo, taken up in 5 ml of DCM, and purified on silica gel 5-50% DCM/EtOAc to give 1-(3-(methylamino)-1-trityl-1H-pyrazolo[4,3-c]pyridin-6-yl)-3-(phenyl(tetrahydrofuran-2-yl)methyl)urea. MS ESI calc'd. for C38H37N6O2 [M+H]+ 609. found 609.

1. customThe vial was evacuated
2. additionback-filled with N2 (×3)
3. customRoom temperature
4. customThe crude reaction mixture
5. filtrationfiltered through celite
6. concentrationThe filtrate was concentrated in vacuo
7. custompurified on silica gel 5-50% DCM/EtOAc