反应详情

温度

55 °C

To a solution of 6-(4-chlorophenyl)-5-(phenyl)-2-oxo-1,2-dihydropyridine-3-nitrile (200 mg, 0.65 mmol) from Example 1, Step B in DMF (3 mL) was added benzyl bromide (0.10 mL, 0.85 mmol) and then cesium carbonate (276 mg, 0.85 mmol). The reaction was stirred at 55° C. for 3 h and was then diluted with water and extracted twice with methylene chloride. The organic layers were washed with a portion of brine and the combined organic layers were dried over anhydrous sodium sulfate and concentrated in vacuo. The products were separated by preparative TLC (30% ethyl acetate in hexanes) to give the desired higher Rf O-alkylation title product.

1. extractionextracted twice with methylene chloride
2. washThe organic layers were washed with a portion of brine
3. dry with materialthe combined organic layers were dried over anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe products were separated by preparative TLC (30% ethyl acetate in hexanes)