反应详情

250 ml of water and 300 ml of cyclohexylamine were put into a 1-liter balloon flask. 139 g of moist 7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid were added by fractions, the temperature being maintained at from 20°-30° C. The mixture was stirred at room temperature for three hours and then the solution was treated with 30 g of black carbon 3S. After filtration, 300 ml of hydrochloric acid (d=1.18) were added. The precipitate was recrystallized, washed with water and dried. 92 g of 7-cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 150° C.).

1. temperaturethe temperature being maintained at from 20°-30° C
2. additionthe solution was treated with 30 g of black carbon 3S
3. filtrationAfter filtration, 300 ml of hydrochloric acid (d=1.18)
4. additionwere added
5. customThe precipitate was recrystallized
6. washwashed with water
7. customdried