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Ammonia → HCID 21520060, Verbindung

HRID 1282786
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1282786
[CH2:1]([S:8][C:9]1[CH:10]=[C:11]([CH:15]=[C:16]([S:25](Cl)(=[O:27])=[O:26])[C:17]=1[O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:12]([OH:14])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH3:29]>>[CH2:1]([S:8][C:9]1[CH:10]=[C:11]([CH:15]=[C:16]([S:25](=[O:27])(=[O:26])[NH2:29])[C:17]=1[O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:12]([OH:14])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 222AmmoniaHCID 21520076HCID 21520076, Verbindung

Produkt 1

HCID 21520060HCID 21520060, Verbindung

Versuchsvorschrift

3-Benzylthio-5-chlorosulfonyl-4-phenoxybenzoic acid (0.6 g) is added to concentrated aqueous ammonia (10 ml). After 1 hour, the reaction mixture is heated on a steam-bath for 15 minutes, and crude 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid until pH 2.5. The crude product is dissolved in aqueous sodium hydrogen carbonate by heating. After cooling, the precipitated sodium salt of 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration. The salt is redissolved in hot water (20 ml) and 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid. After cooling and collecting by filtration, and drying in vacuo at 80°C, the compound is obtained with a melting point of 235°-236°C.

Aufarbeitung

  1. temperaturethe reaction mixture is heated on a steam-bath for 15 minutes
  • customcrude 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid until pH 2.5
  • dissolutionThe crude product is dissolved in aqueous sodium hydrogen carbonate
  • temperatureby heating
  • temperatureAfter cooling
  • filtrationthe precipitated sodium salt of 3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid is collected by filtration
  • dissolutionThe salt is redissolved in hot water (20 ml)
  • custom3-benzylthio-4-phenoxy-5-sulfamylbenzoic acid precipitated by addition of 1 N hydrochloric acid
  • temperatureAfter cooling
  • filtrationcollecting by filtration
  • customdrying in vacuo at 80°C
  • customthe compound is obtained with a melting point of 235°-236°C.
  • Quellen und Nachweise

    ORD-Eintrag
    ord-b20ad1298a4949c9b3a675d1b5f7e76b
    Quelldatensatz
    uspto-grants-1976_08
    DOI
    10.6084/m9.figshare.5104873.v1
    Patentnummer
    US03972886

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