反应详情

N-(1-ethoxy-ethylidene)-benzamide 400 mg (2.09 mmol) was dissolved in a mixed solvent of dichloromethane 20 ml and methanol 10 ml, and (4-methylsulfanyl-phenyl)-hydrazine hydrochloride 439 mg (2.23 mmol) was added to the solution. Then, triethylamine 0.35 ml (2.51 mmol) was slowly added dropwise at room temperature for 10 minutes and stirred for 8 hours. After completing the reaction, water 20 ml was added to the reacting solution and extracted two times with dichloromethane, and then, the collected organic layer was washed with saturated brine. The organic layer was dried with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure, and the resulting product was purified through a flash column chromatography (ethyl acetate:normal hexane=1:1). As a result, 3-methyl-1-(4-methylsulfanyl-phenyl)-5-phenyl-1H-[1,2,4]triazole (359 mg, yield: 61%) was obtained as a liquid phase.

1. additionwas added to the solution
2. additionwas added to the reacting solution
3. extractionextracted two times with dichloromethane
4. washthe collected organic layer was washed with saturated brine
5. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customthe resulting product was purified through a flash column chromatography (ethyl acetate:normal hexane=1:1)