反应详情

To a stirred solution of aminoacetaldehyde diethyl acetal (6.66 g, 50.0 mmol) in CH2Cl2 (100 ml) was added triethylamine (5.06 g, 50.0 mmol), 4-bromobenzoyl chloride (10.97 g, 50.0 mmol), and the mixture was stirred for 6 hours. The reaction mixture was concentrated in vacuo. The residue was dissolved in ethyl acetate. The solution was washed with 0.5N HCl aqueous solution, water, saturated NaHCO3 aqueous solution, brine, dried over MgSO4, and concentrated in vacuo. The residue was recrystallized with ethyl acetate-hexane to give title compound (10.45 g, 66% yield). 1H-NMR (CDCl3) δ: 7.65 (d, J=9 Hz, 2H), 7.58 (d, J=9 Hz, 2H), 6.35 (s, 1H), 4.61 (t, J=5 Hz, 1H), 3.81-3.69 (m, 2H), 3.64-3.53 (m, 4H), 1.24 (t, J=7 Hz, 6H).

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate
3. washThe solution was washed with 0.5N HCl aqueous solution, water, saturated NaHCO3 aqueous solution, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was recrystallized with ethyl acetate-hexane