反应详情

A solution of methylamine (6.3 mL, 12.5 mmol) in THF was added to a suspension of 8-nitro-2-(3-(trifluoromethyl)phenyl)-4H-benzo[d][1,3]oxazin-4-one 3 (1.5 g, 4.2 mmol) in AcOH (18 mL). The reaction mixture was heated under gentle reflux for 12 h then cooled to room temperature. The volatiles were removed in vacuo and the residue was taken up in EtOAc, washed with sat. aq NaHCO3, brine, dried (MgSO4) and concentrated. The residue was purified by MPLC eluting with pentane/EtOAc (0-75%) to give 4 (1.3 g, 89% yield) as a yellow solid.

1. temperatureThe reaction mixture was heated
2. temperatureunder gentle reflux for 12 h
3. customThe volatiles were removed in vacuo
4. washwashed with sat. aq NaHCO3, brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customThe residue was purified by MPLC
8. washeluting with pentane/EtOAc (0-75%)