Acetone → HCID 131711713, Verbindung

HRID 1660038Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1660038
[CH:1]1([NH:7][S:8]([C:11]2[CH:12]=[C:13]([C:21]([OH:23])=O)[C:14]3[O:19][CH2:18][CH2:17][O:16][C:15]=3[CH:20]=2)(=[O:10])=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.ClC(OC[CH:30]([CH3:32])C)=O.C([NH:35]CC)C.C[C:39]([CH3:41])=O>C(N(CC)CC)C>[CH2:39]([C:20]1[C:15]2[O:16][CH2:17][CH2:18][O:19][C:14]=2[C:13]([C:21]([NH2:35])=[O:23])=[C:12]([CH2:30][CH3:32])[C:11]=1[S:8](=[O:9])(=[O:10])[NH:7][CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1)[CH3:41]

Komponenten

7

Edukt 5

HCID 180AcetoneHCID 962WaterHCID 8021DiethylamineHCID 62365Isobutyl chloroformateHCID 205447497-Cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid

Produkt 1

HCID 131711713HCID 131711713, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-28eb3def46f349a7887845fd68ca24f8
Quelldatensatz
uspto-grants-1981_12
Patentnummer
US04306072

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