反应详情

温度

80 °C

A mixture of 4-chloro-5H-pyrrolo[3,2-d]pyrimidine (307 mg), [5-amino-2-(benzyloxy)phenyl]methanol (459 mg) and N,N-dimethylformamide (10 mL) was stirred at 80° C. for 4 hrs. The reaction mixture was concentrated under reduced pressure, aqueous sodium hydrogen carbonate solution was added and the mixture was extracted with ethyl acetate containing tetrahydrofuran. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (eluent, methanol:ethyl acetate=0:100→30:70). Ethanol and ethyl acetate were added and the precipitate was collected by filtration to give the title compound (279 mg) as a brown powder.

1. concentrationThe reaction mixture was concentrated under reduced pressure, aqueous sodium hydrogen carbonate solution
2. additionwas added
3. extractionthe mixture was extracted with ethyl acetate
4. additioncontaining tetrahydrofuran
5. washThe extract was washed with saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customThe solvent was evaporated under reduced pressure
8. customthe obtained residue was purified by silica gel column chromatography (eluent, methanol:ethyl acetate=0:100→30:70)
9. additionEthanol and ethyl acetate were added
10. filtrationthe precipitate was collected by filtration