反应详情

温度

140 °C

A mixture of 2-hydrazinylbenzoic acid hydrochloride (1.05 g, 5.57 mmol), (E)-ethyl 2-cyano-3-ethoxyacrylate (0.9 g, 5.32 mmol) and sodium acetate (0.457 g, 5.57 mmol) in DMF (7 mL) was heated to 140° C. for 2 h then cooled. Water (5 mL) was added and the mixture was stirred at rt for 1 h then filtered. The solid was washed with H2O, EtOH and Et2O then dried. The solid was dissolved in EtOH (10 mL), treated with a 1M solution of sodium hydroxide (23 mL, 23 mmol) and the mixture was heated at 80° C. for 18 hr. The mixture was filtered hot then cooled and acidified with acetic acid and 10% HCl. The precipitated product was filtered, washed with H2O and Et2O, dried well and used without any further purification.

1. temperaturethen cooled
2. filtrationthen filtered
3. washThe solid was washed with H2O, EtOH and Et2O
4. customthen dried
5. dissolutionThe solid was dissolved in EtOH (10 mL)
6. temperaturethe mixture was heated at 80° C. for 18 hr
7. filtrationThe mixture was filtered hot
8. temperaturethen cooled
9. filtrationThe precipitated product was filtered
10. washwashed with H2O and Et2O
11. customdried well
12. customused without any further purification