反应详情

A solution of 1-benzyl-3-(tritylamino)-2-azepanone (425 mg, 0.922 mmol) in tetrahydrofuran (11 ml) was added dropwise to a suspension of lithium aluminum hydride (140 mg, 3.69 mmol) in tetrahydrofuran (22 ml) at room temperature, and the resulting mixture was stirred for 30 minutes and then refluxed for 3 hours. After the reaction mixture was cooled, water (0.14 ml), a 2N-aqueous sodium hydroxide solution (0.3 ml) and water (0.14 ml) were added thereto under ice-cooling. The resulting mixture was filtered and the solvent of the filtrate was distilled off under reduced pressure. The resulting residue was purified by a silica gel column chromatography (eluent: chloroform/methanol) to obtain 1-benzyl-N-trityl-3-azepanamine (319 mg, 78%).

1. temperaturerefluxed for 3 hours
2. temperatureAfter the reaction mixture was cooled
3. temperatureunder ice-cooling
4. filtrationThe resulting mixture was filtered
5. distillationthe solvent of the filtrate was distilled off under reduced pressure
6. customThe resulting residue was purified by a silica gel column chromatography (eluent: chloroform/methanol)