反应详情

温度

1 °C

To a solution of 2-(3,4-dimethoxy-phenylamino)-9-iodo-5H,7H-benzo[b]pyrimido[4,5-d]azepin-6-one (I-30) (100 mg, 0.210 mmol) in 4 mL anhydrous DMF at room temperature was added zinc cyanide (14 mg, 0.120 mmol), tris(dibenzylideneacetone)dipalladium (9.5 mg, 0.01 mmol), 1,1′-bis(diphenyl-phosphino)ferrocene (14.0 mg, 0.02 mmol) and a drop of H2O. The solution was degassed with argon then stirred at 1° C. for 16 h. The solution was allowed to cool to 22° C., then diluted with EtOAc and saturated aqueous sodium bicarbonate. The organic layer was then washed with H2O and brine, dried over Na2SO4, and concentrated in vacuo. The product was recrystallized in methanol and CH2Cl2 to give I-92 (92%): MS Rt=2.49 min, m/z=388 (M+H).

1. customThe solution was degassed with argon
2. temperatureto cool to 22° C.
3. additiondiluted with EtOAc and saturated aqueous sodium bicarbonate
4. washThe organic layer was then washed with H2O and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe product was recrystallized in methanol
8. customCH2Cl2 to give I-92 (92%)