反应详情

LiAlH4 in THF (1 M, 6.58 mL) is added to a solution of 6-fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine (0.8 g) in THF (10 mL) at 00 C. and then stirred at rt overnight. The reaction mixture is quenched with a few drops of water followed by addition of EtOAc (10 mL). The solid is filtered off and washed with EtOAc (15 mL). The filtrate is concentrated in vacuo and the residue is purified by silica gel column chromatography eluting with 15% EtOAc in heptane to afford 6-fluoro-2,3-dihydro-benzo[1,4]oxazin-4-ylamine (0.44 mg).

1. customThe reaction mixture is quenched with a few drops of water
2. additionfollowed by addition of EtOAc (10 mL)
3. filtrationThe solid is filtered off
4. washwashed with EtOAc (15 mL)
5. concentrationThe filtrate is concentrated in vacuo
6. customthe residue is purified by silica gel column chromatography
7. washeluting with 15% EtOAc in heptane