反应详情

5-Methylsulfanyl-2H-[1,2,4]triazol-3-ylamine (0.216 g, 1.7 mmol) was taken in dry DMF (15 ml) and dry potassium carbonate (800 mg) and KI (20 mg) was added to it and the reaction mixture stirred at room temperature 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 then quenched with water and extracted with ethyl acetate. Drying of the organic layer with Na2SO4 followed by concentration afforded crude product that was purified by column chromatography (CHCl3/MeOH): 1H NMR (300 MHz, DMSO-d6): δ 7.24 (d, 2H), 6.98 (d, 2H), 6.24 (s, 2H), 4.84 (s, 2H), 3.57 (m, 4H), 3.21 (m, 2H), 3.13 (m, 2H), 2.37 (s, 3H).

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 crude product that
8. customwas purified by column chromatography (CHCl3/MeOH)