反应详情

Add sodium hydride (1 g, 42.1 mmol) to a stirred solution of (2-bromo-4-fluoro-phenyl)-acetonitrile (3 g, 14 mmol) in 10 mL of dimethyl formamide (DMF) at 0° C. Stir the mixture at 0° C. to RT for half an hour. Add methyl iodide (6 g, 42 mmol). Stir for another 30 min. Quench the reaction with water. Extract the product into DCM. Dry the organic phase over sodium sulfate and concentrate to give an oily residue. Purify the residue by flash column chromatography (FCC) (hexane to 20% ethyl acetate in hexane as gradient elute) to give the title compound as a white solid (2.2 g, 65%). 1H NMR (400 MHz, CDCl3) δ 7.41-7.47 (m, 2H), 7.03-7.08 (m, 1H), 1.88 (s, 6H).

1. stirringStir for another 30 min
2. customQuench
3. customthe reaction with water
4. extractionExtract the product into DCM
5. dry with materialDry the organic phase over sodium sulfate
6. concentrationconcentrate
7. customto give an oily residue
8. customPurify the residue
9. washby flash column chromatography (FCC) (hexane to 20% ethyl acetate in hexane as gradient elute)