反应详情

To a solution of (2R,5S)-1-benzyl-2,5-dimethylpiperazine (3.52 g, 17.2 mmol) in tetrahydrofuran (50 mL), trimethylamine (2.12 g, 20.9 mmol) and di-tert-butylcarbonate (4.56 g, 20.9 mmol) were added under ice-cold conditions, and the mixture was stirred for 15 minutes. Then, the mixture was stirred at room temperature for 5.5 hours. The reaction solution was added water, extracted with ethyl acetate, washed with brine, dried over sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate), and the title compound (3.16 g, 60%) was obtained as a pale yellow oil.

1. stirringThen, the mixture was stirred at room temperature for 5.5 hours
2. extractionextracted with ethyl acetate
3. washwashed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate)