反应详情

温度

10 °C

34.1 g of 7-cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid, 35 ml of water and 10.5 g of triethylamine were introduced into a 250 ml balloon flask provided with a stirrer and a thermometer. 100 ml of acetone were added and the mixture was cooled to 10° C. 14 g of isobutyl chloroformate were added and the mixture was maintained under stirring for 30 minutes at room temperature. 8 g of diethylamine were introduced at a temperature of from 15°-20° C. After stirring for three hours, the solvent was removed under vacuum. The residue was washed with water, dried, dissolved in 180 ml of absolute ethanol and treated with 3 g of black carbon. After filtration and crystallization, 23 g of diethyl-7-cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxamide were obtained (M.P.: 201° C.). The structure was confirmed by infrared and nuclear magnetic resonance analyses.

1. customprovided with a stirrer
2. temperaturethe mixture was maintained
3. stirringAfter stirring for three hours
4. customthe solvent was removed under vacuum
5. washThe residue was washed with water
6. customdried
7. dissolutiondissolved in 180 ml of absolute ethanol
8. additiontreated with 3 g of black carbon
9. filtrationAfter filtration and crystallization