反应详情

温度

100 °C

To an oven-dried 250 mL round bottom flask was added 2-amino-6-chloro-9-(trans-4-methoxycyclohexyl)-7H-purin-8(9H)-one (crude, 3.65 g, 12.28 mmol, 1 equiv.) in anhydrous toluene (50 mL), then freshly grounded cesium carbonate (6 g, 18.43 mmol, 1.5 equiv.) with stirring at room temperature under Ar. Pd(OAc)2 (1.24 g, 1.84 mmol, 0.15 equiv.), racemic BINAP (2.67 g, 4.3 mmol, 0.35 equiv.) and 3-bromo-4-nitro-benzonitrile (3.6 g, 15.96 mmol, 1.3 eq) were all added as solids. The reaction was performed under a flow of Argon, with heating at 100° C. for two days. The reaction mixture was cooled to room temperature, then concentrated in vacuo and the resulting residue was purified using flash chromatography (silica gel, gradient elution 10% EtOAc in hexanes to 50% EtOAc in hexanes) to give the desired product as an orange solid (50% yield). MS (EI) m/z 444 (MH)+.

1. additionall added as solids
2. temperatureThe reaction mixture was cooled to room temperature
3. concentrationconcentrated in vacuo
4. customthe resulting residue was purified
5. washflash chromatography (silica gel, gradient elution 10% EtOAc in hexanes to 50% EtOAc in hexanes)