反应详情

To a suspension of 1-methylpiperazine dihydrochloride (8.5 g, 49.2 mmol) and triethylamine (22.8 mL, 164.0 mmol) in THF (150 mL) was added tert-butyl 2-bromoacetate (8.0 g, 41.0 mmol). The mixture was stirred at room temperature for 12 hours. The reaction mixture was diluted with EtOAc (200 mL) and H2O (100 mL). The organic phase was washed with brine, dried (MgSO4), filtered and concentrated to dryness. The residue was purified by column chromatography (silica, 0-10% MeOH in CH2Cl2) to afford the sub-title compound (6.0 g, 69%).

1. washThe organic phase was washed with brine
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated to dryness
5. customThe residue was purified by column chromatography (silica, 0-10% MeOH in CH2Cl2)