反应详情

To a stirred solution of diethyl[(6-bromo-2-cyanoquinolin-7-yl)(difluoro)methyl]phosphonate (370 mg, 0.883 mmol) in dichloromethane (9) at 0° C. was added dropwise bromotrimethylsilane (1.15 mL, 8.83 mmol). The reaction mixture was stirred at room temperature overnight. It was concentrated to dryness, and co-evaporated with dichloromethane (2×). Ethanol (5 mL) was added to the residue, which was stirred for 20 minutes. It was concentrated to dryness and co-evaporated with ethanol (2×). The residue was dissolved in methanol (8 mL) and 2.0 M ammonia in methanol (4.4 mL, 8.80 mmol) was added dropwise. It was stirred for 20 minutes, concentrated to dryness and suspended in diethyl ether. The precipitate was filtered to afford diammonium[(6-bromo-2-cyanoquinolin-7-yl)(difluoro)methyl]phosphonate.

1. concentrationIt was concentrated to dryness
2. additionEthanol (5 mL) was added to the residue, which
3. stirringwas stirred for 20 minutes
4. concentrationIt was concentrated to dryness and co-evaporated with ethanol (2×)
5. dissolutionThe residue was dissolved in methanol (8 mL)
6. stirringIt was stirred for 20 minutes
7. concentrationconcentrated to dryness
8. filtrationThe precipitate was filtered