反应详情

816 mg (6 mmol) of 4-hydroxyacetophenone, 251 mg (1.5 mmol) of 4-[2-chloroethyl]-1H-imidazole hydrochloride, 500 mg (3.6 mmol) of potassium carbonate and sodium iodide (catalyst) are stirred at 80° C. for 5 days in 5 ml of dimethylformamide. The reaction mixture is cooled, filtered and the filtrate is evaporated under reduced pressure to give an oily residue, from which 4-hydroxyacetophenone is extracted with ether at pH=1. Subsequent extraction with ethyl acetate at pH=9 gives the title compound. The latter was treated with oxalic acid in 2-propanol to give the oxalate of the title compound which is crystallized from a methanol/ether (10/1) mixture, M.p.: 178°-182° C.

1. temperatureThe reaction mixture is cooled
2. filtrationfiltered
3. customthe filtrate is evaporated under reduced pressure
4. customto give an oily residue
5. extractionfrom which 4-hydroxyacetophenone is extracted with ether at pH=1
6. extractionSubsequent extraction with ethyl acetate at pH=9