反应详情

To a solution of 1.02 g (7.23 mmol) of 1H-1,2,4-triazole-3-carboxylic acid ethyl ester in 6 ml of DMF was added 1.46 g (1.44 mmol) of triethylamine. To the solution was added dropwise with stirring under ice-cooling 1.14 g (7.94 mmol) of dimethylsulfamoyl chloride. The mixture was stirred at room temperature for 8 hours. 30 ml of Water was added thereto and extracted with 20 ml of ethylacetate. The extract was washed with a saturated aqueous solution of sodium hydrogencarbonate and water, dried over Na2SO4 and evaporated under reduced pressure to give an oil. The obtained oil was purified with silica gel chromatography (eluate: hexane/ethylacetate=2:1) to give 1.46 g of 1-dimethylsulfamoyl-1,2,4-triazole-3-carboxylic acid ethyl ester as a white crystal. Yield: 82%.

1. additionTo the solution was added dropwise
2. stirringThe mixture was stirred at room temperature for 8 hours
3. extractionextracted with 20 ml of ethylacetate
4. washThe extract was washed with a saturated aqueous solution of sodium hydrogencarbonate and water
5. dry with materialdried over Na2SO4
6. customevaporated under reduced pressure
7. customto give an oil
8. customThe obtained oil was purified with silica gel chromatography (eluate: hexane/ethylacetate=2:1)