反応 #40703

反応方程式

ethyl 2-chloronicotinate

4-phenylimidazole

K2CO3

→

dark oil

収率 28.9%

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

収率 28.9%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   濃縮by concentrating
2. 2
   洗浄washing with water and sat. NaCl solution
3. 3
   乾燥drying over MgSO4
4. 4
   ろ過filtering
5. 5
   その他evaporating

実験手順

A mixture of 5.0 g of ethyl 2-chloronicotinate (26.94 mmol), 3.4 g of 4-phenylimidazole (23.58 mmol), 7.6 g of K2CO3 and 80 mg of 18-crown-6 in 18 ml of N,N-dimethylformamide was heated in a microwave at 160° C. for about 1 hour. This was followed by concentrating, taking up the residue in dichloromethane, washing with water and sat. NaCl solution, drying over MgSO4, filtering and evaporating. Chromatography on silica gel (eluent: CH2Cl2/methanol 2%-5%) resulted in 2 g of a dark oil, which was immediately reacted further; ESI-MS [M+H]+=294.15.

出典