Diethylamine → HCID 20544715, Verbindung

HRID 127430

Reaktionsgleichung

Reaktionsgleichung von HRID 127430
[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 20544715HCID 20544715, VerbindungAusbeute 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-c69e82d1a6f249228d143e5e479bf5e1
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255580

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