反应详情

温度

70 °C

To a solution of 1-bromo-2-bromomethyl-3-nitro-benzene (3.39 g, 11.53 mmol) in DMF (50 nml) was added KOAc (7.6 g, 77.4 mmol). The reaction was heated at 70° C. for an hour. After cooling to room temperature, the mixture was partitioned between water and ethyl acetate. The organic layer was washed with water and brine, and dried over MgSO4 Acetic acid 2-bromo-6-nitro-benzyl ester (3.1 g) was obtained as a brown oil after concentration under vacuum (˜100%). 1H NMR (CDCl3, 300 MHz) δ: 2.06(s, 3H), 5.46 (s, 2H), 7.377(t, J=8.1 Hz), 7.778(dd, J=1.23 Hz, 8.14 Hz), 7.856(dd, J=1.23 Hz, 8.07 Hz).

1. temperatureAfter cooling to room temperature
2. customthe mixture was partitioned between water and ethyl acetate
3. washThe organic layer was washed with water and brine
4. dry with materialdried over MgSO4 Acetic acid 2-bromo-6-nitro-benzyl ester (3.1 g)
5. customwas obtained as a brown oil
6. concentrationafter concentration under vacuum (˜100%)