反应详情

To a suspension of LiAlH4 (6.0 mmol, 0.23 g) in 25.0 mL of Et2O was added a solution of 5-(3,4-difluoro-phenyl)-morpholin-3-one (2.0 mmol, 0.42 g) in 20.0 mL Et2O and 5.0 mL THF at room temperature. The resulting suspension was heated to reflux for 2 hours and was then quenched with water and aq. NaOH solution. The solid was filtered off and the filtrate was dried over Na2SO4. The filtrate was then decanted and the solvent was removed in vacuo to obtain 5-(3,4-difluoro-phenyl)-morpholine as a viscous oil. It was converted to its hydrochloride salt for its analysis. Yellow powder. M.P.=171-173° C.; Mass spec. 200 (M+1, 100%). Analysis calculated for C10H12NOF2Cl.0.5 acetone: C, 51.96; H, 5.61; N, 5.41. Found: C, 51.98; H, 5.70; N, 5.34.

1. temperatureThe resulting suspension was heated
2. temperatureto reflux for 2 hours
3. customwas then quenched with water and aq. NaOH solution
4. filtrationThe solid was filtered off
5. dry with materialthe filtrate was dried over Na2SO4
6. customThe filtrate was then decanted
7. customthe solvent was removed in vacuo