Cyclohexylamine → 7-Cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid

HRID 2052665Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2052665
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[S:9]([C:12]1[CH:13]=[C:14]([C:22]([OH:24])=[O:23])[C:15]2[O:20][CH2:19][CH2:18][O:17][C:16]=2[CH:21]=1)(=[O:11])=[O:10]>O>[CH:1]1([NH:7][S:9]([C:12]2[CH:13]=[C:14]([C:22]([OH:24])=[O:23])[C:15]3[O:20][CH2:19][CH2:18][O:17][C:16]=3[CH:21]=2)(=[O:11])=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 7965CyclohexylamineHCID 64553167-(Chlorosulphonyl)-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid

Produkt 1

HCID 205447497-Cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

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.).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-34783c4a9abd4bfb915df1141d7af870
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04186135

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