反応 #792162

反応方程式

potassium carbonate

2,3-dichloropyridine

3-chloropyrazole

product

3-Chloropyrazole

→

title product

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

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   温度The reaction mixture was cooled to room temperature
2. 2
   ろ過The precipitated solids were filtered
3. 3
   洗浄washed with water
4. 4
   ろ過The solid filter cake
5. 5
   乾燥dried over magnesium sulfate
6. 6
   濃縮concentrated
7. 7
   その他The crude solid was chromatographed on silica gel using 20% ethyl acetate/hexane as eluent

実験手順

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 the title product as a white solid (39.75 g).

出典