反应详情

240 mg (60% in oil, 6 mmol) of sodium hydride are added slowly to a solution of 1.67 g (12 mmol) of 3-nitrophenol in 10 ml of dimethylformamide and the mixture is stirred at room temperature for 1 hour. 200 mg (1.2 mmol) of 4-(2-chloroethyl)-1H-imidazole hydrochloride and tetrabutylammonium iodide (catalyst) are added and the mixture is stirred at 80° C. for 3 days. The reaction mixture is cooled and 150 ml of diethyl ether are added. The precipitate is separated by filtration and the filtrate is evaporated under reduced pressure to give a residue which is purified by preparative high performance chromatography. The title compound is converted to the oxalate and crystallized from ethanol, M.p.: 174°-178° C.

1. stirringthe mixture is stirred at 80° C. for 3 days
2. temperatureThe reaction mixture is cooled
3. customThe precipitate is separated by filtration
4. customthe filtrate is evaporated under reduced pressure
5. customto give a residue which
6. customis purified by preparative high performance chromatography
7. customcrystallized from ethanol, M.p.: 174°-178° C.