反应详情

温度

0 °C

Pyridinecarboxaldehyde (0.95 ml, 10 mmol) is added into a reaction flask containing 20 ml of methylene chloride and ethylene diamine (0.78 ml, 10.5 mmol) is added. After the reaction is carried out at 0° C. for 20 minutes, N-bromosuccinimide (1.87 g, 10.5 mmol) is added. The reaction temperature is slowly raised from 0° C. to the room temperature and the reaction is further carried out for 24 hrs at the room temperature. 10% sodium hydroxide solution is added to have the solution become alkaline. After extraction with a small amount of methylene chloride is carried out for 2 times, the organic layer is collected and concentrated to obtain white solids. After purified by silicone chromatographic column, the product pyil is obtained. The yield is about 90%. 1H NMR (400 MHz, CDCl3): δ 8.55-8.54 (m, 1 H), 8.11 (d, 1 H, J=7.6 Hz), 7.76-7.71 (m, 1 H), 7.34-7.21 (m, 1 H), 3.82 (s, 4 H).

1. additionis added
2. waitthe reaction is further carried out for 24 hrs at the room temperature
3. extractionAfter extraction with a small amount of methylene chloride
4. customthe organic layer is collected
5. concentrationconcentrated
6. customto obtain white solids
7. customAfter purified by silicone chromatographic column
8. customthe product pyil is obtained