反应详情

To a solution of 5-(4-bromo-2-formyl-N-methylanilino)pentanoic acid (3.0 g) in DMF(8 ml), potassium carbonate (1.6 g) and a solution of methyl iodide/DMF (1.6 g/2 ml) were added at room temperature, and the resulting mixture was stirred for 2 hours. Ethyl acetate and water were added to the mixture, and the organic layer was separated, washed with water, dried over anhydrous sodium sulfate, and concentrated to give yellow oil of 5-(4-bromo-2-formyl -N-methylanilino)pentanoic acid methylester (3.0 g, yield 97%). 1H-NMR(CDCl3, δ, 300 MHz): 1.58-1.64(4H, m), 2.28(2H, t, J=6.8 Hz), 2.83(3H, s), 3.09(2H, t, J=6.8 Hz), 3.63(3H, s), 6.95(1H, d, J=8.8 Hz), 7.51(1H, dd, J=8.8, 2.4 Hz), 7,83(1H, d, J=2.4 Hz), 10.14(1H, s). FAB-MS ([M+Na]+): 350. IR(neat, cm−1): 1735, 1681.

1. customthe organic layer was separated
2. washwashed with water
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated