反应详情

5-(2-Bromo-phenyl)-1H-tetrazole (0.374 g, 1.66 mmol) was taken in dry DMF (15 mL) and dry potassium carbonate (800 mg) and KI (20 mg) was added to it and stirred at rt for 1 h under nitrogen. 2-Chloro-1-[4-(4-chloro-phenyl)-piperazin-1-yl]-ethanone (500 mg, 1.8 mmol) in DMF (5 mL) was then added to the mixture through a syringe. The reaction was then heated at 140° C. for 14 h, cooled and quenched with water and extracted with ethyl acetate. Drying of the organic layer with Na2SO4 followed by concentration afforded material that was further purified by flash column chromatography (ethyl acetate/pet ether): 1H NMR (300 MHz, CDCl3): δ 7.90 (d, 1H), 7.74 (d, 1H), 7.45 (t, 1H), 7.35 (t, 1H), 7.25 (d, 2H), 6.87 (d, 2H), 5.65 (s, 2H), 3.84 (m, 2H), 3.73 (m, 2H), 3.20 (m, 4H).

1. temperatureThe reaction was then heated at 140° C. for 14 h
2. temperaturecooled
3. customquenched with water
4. extractionextracted with ethyl acetate
5. dry with materialDrying of the organic layer with Na2SO4
6. concentrationfollowed by concentration
7. customafforded material that
8. customwas further purified by flash column chromatography (ethyl acetate/pet ether)