Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetone | HCID 180 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | Diethylamine | HCID 8021 | — |
| Edukt | Isobutyl chloroformate | HCID 62365 | — |
| Edukt | 7-Cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid | HCID 20544749 | — |
| Lösungsmittel | Triethylamine | HCID 8471 | — |
| Produkt | HCID 131711713 | HCID 131711713 | — |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US04306072 |
|---|
| Quelldatensatz | uspto-grants-1981_12 |
|---|
| ORD ID | ord-28eb3def46f349a7887845fd68ca24f8 |
|---|
| Quellennotiz | uspto-grants-1981_12 |
|---|