反应详情

To a solution of ethyl 2-chloro-6-(trifluoromethyl)isonicotinate (0.200 g, 0.789 mmol, Anichem) in tetrahydrofuran (5 mL) at 0° C. was added 3.0M methylmagnesium bromide in diethyl ether (0.66 mL, 2.0 mmol). After 30 minutes, the reaction was quenched by the addition of saturated ammonium chloride solution and extracted with three portions of ethyl acetate. The combined extracts were dried over sodium sulfate, decanted and concentrated. Used without further purification in Step B. 1H NMR (300 MHz, CDCl3) δ 7.70 (d, J=1.4 Hz, 1H), 7.66-7.59 (m, 1H), 1.59 (s, 6H); 19F NMR (282 MHz, CDCl3) 5-68.30 (s); LCMS (M+H)+: 240.1.

1. customthe reaction was quenched by the addition of saturated ammonium chloride solution
2. extractionextracted with three portions of ethyl acetate
3. dry with materialThe combined extracts were dried over sodium sulfate
4. customdecanted
5. concentrationconcentrated
6. customUsed without further purification in Step B