反应详情

To a teflon-lined septum sealed Schlenk tube, a mixture of Compound 11a (1.0 g; 2.7 mmol), pyridin-3-yl boronic acid (0.83 g; 6.75 mmol), Cs2CO3 (2.60 g; 8.1 mmol) and [1,1-Bis(diphenylphosphino)-ferrocene]dichloro-palladium(11) (0.49 g; 0.6 mmol) in a mixture of dioxane (15 mL) and EtOH (1 mL) was irradiated in a microwave reactor at 150° C. for 55 min. The reaction mixture was poured into water, diluted with EtOAc and the solid was collected by filtration. The organic phase was isolated and dried over MgSO4. and the reaction mixture was concentrated under reduced pressure. The resultant residue was purified by reverse phase HPLC, eluting with a CH3CN—H2O (0.5% TFA) gradient to afford Compound 11b (0.72 g; 42% yield based on di-TFA). 1H-NMR (300 MHz, MeOH-d4): δ 9.2 (s, 1H), 8.9 (d, 1H), 8.7 (d, 1H), 8.2 (s, 1H), 8.0 (m, 1H), 7.5 (d, 2H), 7.5-7.3 (m, 6H), 7.2 (m, 2H), 5.2 (s, 2H); MS: m/z 414.2 (M+H)+.

1. customsealed Schlenk tube
2. customwas irradiated in a microwave reactor at 150° C. for 55 min
3. filtrationthe solid was collected by filtration
4. customThe organic phase was isolated
5. dry with materialdried over MgSO4
6. concentrationand the reaction mixture was concentrated under reduced pressure
7. customThe resultant residue was purified by reverse phase HPLC
8. washeluting with a CH3CN—H2O (0.5% TFA) gradient