反应详情

To a solution of ethyl-4-(3-cyanopyridine)glycinate (2.47 g, 12.1 mmol) under nitrogen in EtOH (60 mL) was added sodium ethoxide (0.90 g, 13.3 mmol) and the mixture was heated at reflux for 1 hour. The mixture was allowed to cool to ambient temperature then quenched by the addition of water (3 mL) and saturated ammonium chloride solution (5 mL). The solvent was concentrated in vacuo, to provide a residue that was diluted with water (30 mL), and extracted with EtOAc (2×40 mL). The combined organic layers were dried (Na2SO4), filtered and evaporated to give the title compound as a brown solid (1.35 g, 55%). LCMS (method B): RT=0.61 min, M+H+=206.

1. temperaturethe mixture was heated
2. temperatureat reflux for 1 hour
3. customthen quenched by the addition of water (3 mL) and saturated ammonium chloride solution (5 mL)
4. concentrationThe solvent was concentrated in vacuo
5. customto provide a residue that
6. extractionextracted with EtOAc (2×40 mL)
7. dry with materialThe combined organic layers were dried (Na2SO4)
8. filtrationfiltered
9. customevaporated