反应详情

Imidazole (0.16 g, 2.36 mmol) was dissolved in DMF (1.0 mL) in a CEM 10 mL microwave tube and to this was added NaH (0.09 g, 60% dispersion in mineral oil). The content was stirred at room temperature until no more bubbling was observed (˜10 min). Then (E)-9-(2,6-dimethylstyryl)-2-chloro-N-(4-(dimethylphosphoryl)phenyl)-9H-purin-6-amine (0.12 g, 0.236 mmol) was added. The reaction was heated with microwave (120° C., 10 min). Solvent was removed on rotavapor and the residue was partitioned between EtOAc/water, and the organic layer was separated and dried Na2SO4. The product was purified on ISCO combiFlash (12 g silica gel column, 5% MeOH/DCM): MS [M+H]+ 484.

1. customno more bubbling
2. custom(˜10 min)
3. temperatureThe reaction was heated with microwave (120° C., 10 min)
4. customSolvent was removed on rotavapor
5. customthe residue was partitioned between EtOAc/water
6. customthe organic layer was separated
7. customThe product was purified on ISCO combiFlash (12 g silica gel column, 5% MeOH/DCM)