반응 #531813

반응 방정식

2,3-dichloropyridine

3-(trifluoromethyl)-pyrazole

potassium carbonate

→

desired intermediate

수율 75.1%

3-chloro-2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]pyridine

수율 75.1%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도The reaction was cooled to 100° C.
2. 2
   여과filtered through Celite® diatomaceous filter aid
3. 3
   기타to remove solids
4. 4
   기타N,N-Dimethylformamide and excess dichloropyridine were removed by distillation at atmospheric pressure
5. 5
   workup.DISTILLATIONDistillation of the product at reduced pressure (b.p. 139-141° C., 7 mm)

실험 절차

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.

출처