反应详情

To a mixture of N-{3-[(2-chloro-9-{[2-(trimethylsilyl)ethoxy]methyl}-9H-purin-6-yl)oxy]phenyl}prop-2-enamide (210 mg, 0.471 mmol) and 1-(1-methylpyrrolidin-3-yl)-1H-pyrazol-4-amine (93.9 mg, 0.565 mmol) in 1,4-dioxane (7.85 mL) were added Pd2(dba)3 (43.0 mg, 10 mol %), Xantphos (27.2 mg, 10 mol %), and cesium carbonate (460 mg, 1.41 mmol). The reaction vial was sealed, then evacuated and back-filled with nitrogen three times. The mixture was subjected to microwave irradiation at 140° C. for 1 hr at normal absorption. After cooling to rt the reaction was diluted with EtOAc and filtered through a glass fiber filter set. The filtrate was concentrated and dried to give the title compound, which was carried forward without further purification, assuming quantitative yield. m/z (APCI+) for C28H37N9O3Si 576.20 (M+H)+.

1. customThe reaction
2. customvial was sealed
3. customevacuated
4. additionback-filled with nitrogen three times
5. customirradiation at 140° C. for 1 hr
6. customat normal absorption
7. additionwas diluted with EtOAc
8. filtrationfiltered through a glass fiber
9. filtrationfilter
10. concentrationThe filtrate was concentrated
11. customdried