반응 #40706

반응 방정식

H2O

ethyl 2-chloronicotinate

4-phenylpyrazole

K2CO3

→

oil

수율 79.8%

Ethyl 2-(4-phenyl-1H-pyrazol-1-yl)pyridine-3-carboxylate

수율 79.8%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   추출after extraction with ethyl acetate
2. 2
   세척the organic phase was washed with H2O and sat. NaCl solution
3. 3
   기타The crude product obtained
4. 4
   기타after drying
5. 5
   기타concentration of the solution was purified by chromatography on silica gel (eluent: CH2Cl2/methanol 1-10%)

실험 절차

A mixture of 3.6 g of ethyl 2-chloronicotinate (19.4 mmol), 1.3 g of 4-phenylpyrazole (8.12 mmol), 4.4 g of K2CO3, 40 mg of 18-crown-6 and 30 mg of KI in 30 ml of N,N-dimethylformamide was stirred at 130° C. for 6 hours. For workup, H2O was added and, after extraction with ethyl acetate, the organic phase was washed with H2O and sat. NaCl solution. The crude product obtained after drying and concentration of the solution was purified by chromatography on silica gel (eluent: CH2Cl2/methanol 1-10%). In total, 1.9 g of an oil were obtained, which crystallized completely on standing in a refrigerator.

출처