反应详情

温度

110 °C

A microwave vial was charged with 7-fluoro-2H-3,1-benzoxazine-2,4(1H)-dione (750 mg, 4.14 mmol) and methyl amine 40% aqueous solution (19.8 mL, 22.8 mmol, 5.5 eq). The reaction was stirred and heated in the microwave for 6 min at 110° C. The aqueous solution was extracted with methylene chloride (3×). Organic layers were combined and washed with 5% NaHCO3 solution and brine, dried over sodium sulfate, then concentrated to give a pale yellow oil that was used without further purification (434 mg, 62% yield). MS: M(C8H9FN2O)=168.17, (M+H)+=169 and (M+H−NHMe)+=138.

1. extractionThe aqueous solution was extracted with methylene chloride (3×)
2. washwashed with 5% NaHCO3 solution and brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated
5. customto give a pale yellow oil that
6. customwas used without further purification (434 mg, 62% yield)