反应详情

To a solution of 8-Fluoro-2,2-dimethyl-6-nitro-2H-benzo[b][1,4]oxazin-3(4H)-one (0.75 g, 3.1 mmol) in 25 ml anhydrous THF, P2S5 (2.8 g, 6.25 mmol) was added and the reaction mixture was heated to reflux for 12 hours. Analysis of LC-MS indicated the completion of the reaction. Volatiles were removed in vacuo and the crude reaction mixture was partitioned in EtOAc (100 ml) and saturated aqueous NH4Cl (100 ml). Layers were separated and the organic layer was washed (×2) with saturated aqueous NH4Cl (50 ml). EtOAc layer was dried over Na2SO4 and concentrated to give the product in 69% yield (0.55 g). LCMS (m/z) 257 (MH+).

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 12 hours
3. customthe completion of the reaction
4. customVolatiles were removed in vacuo
5. customthe crude reaction mixture
6. customwas partitioned in EtOAc (100 ml)
7. customLayers were separated
8. washthe organic layer was washed (×2) with saturated aqueous NH4Cl (50 ml)
9. dry with materialEtOAc layer was dried over Na2SO4
10. concentrationconcentrated
11. customto give the product in 69% yield (0.55 g)