反应详情

温度

40 °C

A mixture of 2-bromo-2′-nitroacetophenone (18 g), 4-methoxybenzamidine (20 g), and silica gel (20 g) in acetonitrile (500 ml) is heated at 40° C. for 24 hours. The reaction is evaporated and the residue put on a layer of silica gel and eluted with 50% ethyl acetate/hexane (1500 ml). The solution is evaporated under reduced pressure to approximately 250 ml and extracted with 5% HCl (3×250 ml). The combined aqueous solution is basified with K2CO3 and extracted with ethyl acetate (3×400 ml) to afford 2-(4-methoxyphenyl)-4-(2-nitrophenyl)-imidazole (17 g) as a dark yellow oil which is used in the next step without further purification.

1. customThe reaction is evaporated
2. washthe residue put on a layer of silica gel and eluted with 50% ethyl acetate/hexane (1500 ml)
3. customThe solution is evaporated under reduced pressure to approximately 250 ml
4. extractionextracted with 5% HCl (3×250 ml)
5. extractionextracted with ethyl acetate (3×400 ml)