反应详情

温度

90 °C

In a sealed tube was added 1-(4-(5-benzyl-2-chloro-5H-pyrrolo[3,2-d]pyrimidin-4-yloxy)-3,5-dimethylphenyl)ethanone (111 mg, 0.27 mmol), 4-aminobenzonitrile (129 mg, 1.1 mmol), TFE (1.7 mL) and TFA (0.2 mL, 2.16 mmol). The reaction mixture was stirred at 90° C. for 16 h. Upon completion of the reaction, the resulting mixture was cooled, diluted with water, and washed with EtOAc. The combined organic layers were washed with NaHCO3 and brine; dried over Na2SO4; filtered; and concentrated in vacuo. The crude product was purified by silica gel column chromatography, eluting with hexanes:ethyl acetate (9:1-100% EtOAc), to give the product as an off-white solid (68 mg, 51%).

1. customUpon completion of the reaction
2. temperaturethe resulting mixture was cooled
3. washwashed with EtOAc
4. washThe combined organic layers were washed with NaHCO3 and brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationand concentrated in vacuo
8. customThe crude product was purified by silica gel column chromatography
9. washeluting with hexanes