反応 #156302
ord-b0eb2e618633469b82378bdaed9faf19
反応方程式
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度cooling
- 2温度Under ice-cooling
- 3ろ過the reaction mixture was filtered
- 4濃縮The filtrate was concentrated under reduced pressure
- 5その他The residue was purified by silica gel column chromatography (chloroform/methanol)
実験手順
Under a nitrogen atmosphere, to a mixture of 693 mg of lithium aluminum hydride and 30 mL of tetrahydrofuran was added dropwise a solution of 1.0 g of 1-(piperidin-1-yl)cyclobutanecarbonitrile in 18 mL of tetrahydrofuran under ice-cooling. The reaction mixture was stirred at room temperature for 3 hours. Under ice-cooling, 1.5 mL of water and 1.5 mL of a 15% aqueous sodium hydroxide solution were added dropwise thereto. The mixture was diluted with ethyl acetate and the reaction mixture was filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol) to obtain 932 mg of 1-[1-(piperidin-1-yl)cyclobutyl]methanamine.