Diethylamine → 7-Diethylsulfamoyl-1,4-benzodioxane-5-carboxylic acid

HRID 2285491

Reaktionsgleichung

Reaktionsgleichung von HRID 2285491
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].C(N(CC)CC)C.Cl[S:14]([C:17]1[CH:18]=[C:19]([C:27]([OH:29])=[O:28])[C:20]2[O:25][CH2:24][CH2:23][O:22][C:21]=2[CH:26]=1)(=[O:16])=[O:15]>O>[CH2:1]([N:3]([CH2:4][CH3:5])[S:14]([C:17]1[CH:18]=[C:19]([C:27]([OH:29])=[O:28])[C:20]2[O:25][CH2:24][CH2:23][O:22][C:21]=2[CH:26]=1)(=[O:16])=[O:15])[CH3:2]

Komponenten

5

Edukt 3

HCID 8021DiethylamineHCID 8471TriethylamineHCID 64553167-(Chlorosulphonyl)-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid

Produkt 1

HCID 205447157-Diethylsulfamoyl-1,4-benzodioxane-5-carboxylic acidAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

200 ml of water, 100 ml of diethylamine and 200 ml of triethylamine were introduced into a balloon flask provided with an agitator and a thermometer and then 140 g of 7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid were added in portions, the temperature being maintained at from 20°-30° C. The mixture was agitated at ambient temperature and then 500 ml of water were added. The solution was filtered and treated with 300 ml of hydrochloric acid. The precipitate was dried off, washed and dried. 117 g of 7-diethylsulfamoyl-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 149° C.; yield: 74%).

Aufarbeitung

  1. customprovided with an agitator
  2. temperaturethe temperature being maintained at from 20°-30° C
  3. filtrationThe solution was filtered
  4. additiontreated with 300 ml of hydrochloric acid
  5. customThe precipitate was dried off
  6. washwashed
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c8e01a464187497b8069506ba675cee0
Quelldatensatz
uspto-grants-1982_04
Patentnummer
US04323503

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