反应详情

温度

100 °C

A vial was charged with 2-chloro-4-iodo-3-methylfuro[2,3-c]pyridin-7-amine (100 mg, 0.32 mmol), tert-butyl 4-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl]piperidine-1-carboxylate (140 mg, 0.39 mmol), Cs2CO3(150 mg, 0.48 mmol), Pd(dppf)Cl2 (20 mg, 0.027 mmol, 8 mole %), and 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl (40 mg, 0.080 mmol, 26 mole %) in DME (5 mL) and H2O (0.5 mL). The vial was purged with N2 and heated at 100° C. in a microwave reactor for 1 h. Water (20 mL) was added, and the mixture was extracted with EtOAc (3×20 mL). The combined organic extracts were dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by preparative TLC (EtOAc) to afford 85 mg (62%) of the title compound. 1H NMR (400 MHz, CDCl3): δ 7.67 (s, 1H), 7.48 (s, 1H), 7.39 (s, 1H), 4.66 (s, 2H), 4.23 (m, 4H), 2.85 (m, 1H), 2.14 (m, 2H), 2.10 (m, 1H), 1.94 (s, 3H), 1.87 (m, 1H), 1.41 (s, 9H).

1. customThe vial was purged with N2
2. additionWater (20 mL) was added
3. extractionthe mixture was extracted with EtOAc (3×20 mL)
4. dry with materialThe combined organic extracts were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by preparative TLC (EtOAc)