反应详情

温度

0 °C

To a solution of 4-(3-ethyl-4′-fluoro-biphenyl-4-yl)-2,2,6-trimethylpyran-3,5-dione (0.125 g, 0.35 mmol) in dichloromethane (5 ml) is added triethylamine (0.2 ml, 1.43 mmol) and the reaction mixture is cooled to 0° C. Pivaloyl chloride (0.2 ml, 1.63 mmol) is added slowly at 0° C. and the mixture is stirred at 0° C. for 5 hours. The reaction mixture is diluted with water and extracted with dichloromethane (3×25 ml). The organic extracts are combined, dried over anhydrous sodium sulphate and concentrated under reduced pressure. The residue is purified by column chromatography on silica gel to afford 2,2-dimethyl propionic acid 4-(3-ethyl-4′-fluorobiphenyl-4-yl)-2,2,6-trimethyl-5-oxo-5,6-dihydro-2H pyran-3-yl ester (130 mg) as a white solid.

1. extractionextracted with dichloromethane (3×25 ml)
2. dry with materialdried over anhydrous sodium sulphate
3. concentrationconcentrated under reduced pressure
4. customThe residue is purified by column chromatography on silica gel