反应详情

温度

80 °C

Crude 5-isothiocyanato-3-(trifluoromethyl)picolinonitrile 9 (1.390 g, 6.07 mmol) is placed in a 50 mL round-bottomed flask and 4-(1-cyanocyclobutylamino)-2-fluoro-N-methylbenzamide 10 (0.5 g, 2.022 mmol) is added to the flask. The mixture is left under vacuum (using an oil pump) for 1 hour. N,N-dimethylformamide (DMF) (6 ml) is added, the flask sealed under argon with a stopper and heated to 80° C. in a CEM microwave reactor for 20 hours. Methanol (10 ml) and 2N HCl (6 ml) is added and the mixture is refluxed for 2 hours. The mixture is diluted with water (30 ml) and saturated aqueous NaHCO3 (30 ml) is added. The mixture is extracted with ethyl acetate (3×20 ml).

1. waitThe mixture is left under vacuum (
2. customfor 1 hour
3. customthe flask sealed under argon with a stopper
4. temperaturethe mixture is refluxed for 2 hours
5. additionis added
6. extractionThe mixture is extracted with ethyl acetate (3×20 ml)