反应详情

温度

0 °C

6-Chloronicotinoyl chloride (500 mg, 2.76 mmol) and triethylamine (0.576 ml, 4.13 mmol) were taken-up in THF (13.8 ml) under argon and cooled to 0° C. Dimethylamine hydrochloride (337 mg, 4.13 mmol) was dissolved in THF (2 ml) and added dropwise to the reaction mixture over 15 minutes. The mixture was maintained at 0° C. for 1 hour, warmed to room temperature, and stirred for 15 minutes. The reaction was then diluted with ethyl acetate and washed twice with brine. The aqueous layers were combined and back-extracted twice with ethyl acetate. The organic layers were combined, dried over anhydrous magnesium sulfate, filtered, and concentrated to afford the title compound.

1. additionadded dropwise to the reaction mixture over 15 minutes
2. temperatureThe mixture was maintained at 0° C. for 1 hour
3. temperaturewarmed to room temperature
4. washwashed twice with brine
5. extractionback-extracted twice with ethyl acetate
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated