Reacción #531813
ord-7828509d36134cdb89b22cfb65774069
Ecuación de reacción
2,3-dichloropyridine
3-(trifluoromethyl)-pyrazole
potassium carbonate
→
desired intermediate
Rendimiento 75.1%
3-chloro-2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]pyridine
Rendimiento 75.1%
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Temperatura
117.5°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1TemperaturaThe reaction was cooled to 100° C.
- 2Filtraciónfiltered through Celite® diatomaceous filter aid
- 3Otroto remove solids
- 4OtroN,N-Dimethylformamide and excess dichloropyridine were removed by distillation at atmospheric pressure
- 5workup.DISTILLATIONDistillation of the product at reduced pressure (b.p. 139-141° C., 7 mm)
Procedimiento
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 atmospheric pressure. Distillation of the product at reduced pressure (b.p. 139-141° C., 7 mm) afforded 113.4 g of the desired intermediate as a clear yellow oil.