تفاعل #792158
ord-76c25cfed05f422594497f2dd911cd53
معادلة التفاعل
2,3-dichloropyridine
3-trifluoromethylpyrazole
potassium carbonate
→
title compound
المردود 75.1%
3-chloro-2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]pyridine
المردود 75.1%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
117.5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe reaction was cooled to 100° C.
- 2ترشيحfiltered through Celite® diatomaceous filter aid
- 3أخرىto remove solids
- 4أخرىN,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)
الإجراء التجريبي
To a mixture of 2,3-dichloropyridine (99.0 g, 0.67 mol) and 3-trifluoromethylpyrazole (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 the title compound as a clear yellow oil (113.4 g).