反应详情

温度

117.5 °C

To a mixture of 2,3-dichloropyridine (99.0 g, 0.67 mol) and 3-(trifluoromethyl)pyrazole (83 g, 0.61 mol) in dry N,N-dimethylformamide (300 mL) was added potassium carbonate (166.0 g, 1.2 mol) and the reaction was then heated to 110-125° C. over 48 hours. The reaction was cooled to 100° C. and filtered through Celite® diatomaceous filter aid to remove solids. N,N-Dimethylformamide and excess dichloropyridine were removed by distillation at atomospheric pressure. Distillation of the product at reduced pressure (b.p. 139-141° C., 7 mm) afforded the desired intermediate as a clear yellow oil (113.4 g).

1. temperatureThe reaction was cooled to 100° C.
2. filtrationfiltered through Celite® diatomaceous filter aid
3. customto remove solids
4. customN,N-Dimethylformamide and excess dichloropyridine were removed by distillation at atomospheric pressure
5. distillationDistillation of the product at reduced pressure (b.p. 139-141° C., 7 mm)