反应详情

A mixture of 1-(4-methoxy-phenyl)-piperidin-4-one oxime (4.55 g, 20.6 mmol), “Red-Al®” (70% in toluene, 23.4 ml) and toluene (10 ml) was heated at 140° for 2 h. After cooling, the reaction mixture was poured on H2O (100 ml). Extraction of the solution with CH2Cl2, drying of the organic layer, evaporation of the solvent and purification of the residue by chromatography (SiO2, CH2Cl2—MeOH—aq. NH3 140:10:1) gave 1-(4-methoxy-phenyl)-piperidin-4-yl-amine (3.5 g, 89%, white crystals, MS: m/e=207.2 (M+H+)).

1. temperaturewas heated at 140° for 2 h
2. temperatureAfter cooling
3. additionthe reaction mixture was poured on H2O (100 ml)
4. extractionExtraction of the solution with CH2Cl2
5. dry with materialdrying of the organic layer, evaporation of the solvent and purification of the residue by chromatography (SiO2, CH2Cl2—MeOH—aq. NH3 140:10:1)