반응 #531820

반응 방정식

potassium carbonate

2,3-dichloropyridine

3-chloropyrazole

product

3-chloropyrazole

→

title product

3-chloro-2-(3-chloro-1H-pyrazol-1-yl)pyridine

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled to room temperature
2. 2
   여과The precipitated solids were filtered
3. 3
   세척washed with water
4. 4
   여과The solid filter cake
5. 5
   건조dried over magnesium sulfate
6. 6
   농축concentrated
7. 7
   기타The crude solid was chromatographed on silica gel using 20% ethyl acetate/hexane as eluent

실험 절차

To a mixture of 2,3-dichloropyridine (92.60 g, 0.629 mol) and 3-chloropyrazole (i.e. the product of Step B) (64.44 g, 0.629 mol) in N,N-dimethylformamide (400 mL) was added potassium carbonate (147.78 g, 1.06 mol), and the reaction mixture was then heated to 100° C. for 36 hours. The reaction mixture was cooled to room temperature and slowly poured into ice water. The precipitated solids were filtered and washed with water. The solid filter cake was taken up in ethyl acetate, dried over magnesium sulfate and concentrated. The crude solid was chromatographed on silica gel using 20% ethyl acetate/hexane as eluent to afford 39.75 g of the title product as a white solid.

출처