反应详情

温度

80 °C

A mixture of tert-butyl 2-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-5-yl)ethylcarbamate (1.19 g), 3-chloro-4-(3-chlorophenoxy)aniline (1.22 g) and isopropyl alcohol (12.0 mL) was stirred at 80° C. for 15 hrs. Under ice-cooling, aqueous sodium hydrogen carbonate was added, and the mixture was extracted with ethyl acetate. The organic layer washed with brine, and dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (eluent:hexane/ethyl acetate=50/50→100/0), and washed with diisopropyl ether-hexane to give the title compound (1.69 g) as crystals.

1. temperatureUnder ice-cooling
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationThe solvent was concentrated under reduced pressure
6. customthe residue was purified by silica gel chromatography (eluent:hexane/ethyl acetate=50/50→100/0)
7. washwashed with diisopropyl ether-hexane