反应详情

A mixture of 5-(4-cyano-3-fluoro-phenyl)-nicotinic acid ethyl ester from Example 1a, potassium acetate (2 equiv.), and 18-crown-6 ether (2 equiv.) in MeCN is heated at reflux in 36 h. The mixture is cooled, aqueous sodium carbonate is added and stirred at room temperature overnight. The mixture was extracted with ether (discarded). The aqueous layer is neutralized with 1N HCl, extracted with EtOAc, dried over MgSO4, and concentrated. Purification by flash column chromatography gives 5-(4-cyano-3-hydroxy-phenyl)-nicotinic acid ethyl ester.

1. temperatureis heated
2. temperatureat reflux in 36 h
3. temperatureThe mixture is cooled
4. extractionThe mixture was extracted with ether (discarded)
5. extractionextracted with EtOAc
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customPurification by flash column chromatography