反应详情

To a stirred mixture of 4-octyl aniline (0.33 g, 1.6 mmol) and H2O2 (30%, 0.5 ml) in CH3OH (1.5 ml) was added I2 (0.2 g, 0.8 mmol) and the mixture was stirred overnight at room temperature. The solvent was distilled off and the residue was diluted to 10 ml with CH2Cl2, washed with H2O, dried over MgSO4 and filtered. The filtrate was evaporated to dryness to give the title compound (0.46 g, 86%) as yellow paste. 1H NMR (CDCl3) 7.44 (d, 1H, J=1.83 Hz); 6.93 (dd, 1H, J=8.07, 1.86 Hz); 6.65 (d, 1H, J=8.1 Hz); 4.1 (b, 2H); 2.43 (t, 2H, J=7.5 Hz); 1.54-1.49 (m, 2H); 1.26 (b, 10H); 0.87 (t, 3H, J=6.39 Hz).

1. distillationThe solvent was distilled off
2. additionthe residue was diluted to 10 ml with CH2Cl2
3. washwashed with H2O
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customThe filtrate was evaporated to dryness