反应详情

To a solution of 2-aminobenzaldehyde (1.21 g, 10 mmol), and triethylamine (1.39 mL, 10 mmol) in dichloromethane (50 mL) was added propionyl chloride (1.04 mL, 12 mol). The reaction was stirred at room temperature for 3 days. The reaction solution was washed with water and then dried over magnesium sulfate and concentrated in vacuo to yield the crude product (1.65 g, 93%). The product was used without further purification. 1H NMR (400 MHz, CDCl3) δ 11.16 (s, 1H), 9.93 (s, 1H), 8.77 (d, J=8.5 Hz, 1H), 7.67 (d, J=7.7 Hz, 1H), 7.62 (t, J=7.1 Hz, 1H), 7.22 (t, J=7.5 Hz, 1H), 2.51 (q, J=7.6 Hz, 2H), 1.29 (t, J=7.6 Hz, 3H); HPLC ret. time 1.34 min, 10-99% CH3CN, 5 min run; ESI-MS m/z 177.2 (M+1)+.

1. washThe reaction solution was washed with water
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated in vacuo