反应详情

A mixture of (Z)-ethyl 2-cyano-3-ethoxyacrylate (9.64 g, 57.0 mmol), 4-methoxyphenylhydrazine hydrochloride (9.95 g, 57.0 mmol) and Na2CO3 (6.04 g, 57.0 mmol) in EtOH (480 mL) was refluxed for 5 h and stirred overnight at rt. The insoluble material was filtered off and the filtrate was concentrated and solid precipitated. The precipitate was collected and washed with MeOH and washed with water extensively. The pale solid was dried to provide the desired product: 1H NMR (400 MHz, DMSO-D6) δ ppm 7.65 (1H, s), 7.42 (2H, d), 7.07 (2H, d), 6.15 (2H, s), 4.14-4.26 (2H, m), 3.81 (3H, s), 1.27 (3H, t).

1. temperaturewas refluxed for 5 h
2. filtrationThe insoluble material was filtered off
3. concentrationthe filtrate was concentrated
4. customsolid precipitated
5. customThe precipitate was collected
6. washwashed with MeOH
7. washwashed with water extensively
8. customThe pale solid was dried