Sodium Hydroxide → HCID 12138351, Verbindung

HRID 1271666Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1271666
[CH3:1][N:2]([CH3:22])[C:3]([S:5][C:6]1[CH:7]=[C:8]([CH:13]=[C:14]([S:16][C:17](=[O:21])[N:18]([CH3:20])[CH3:19])[CH:15]=1)[C:9]([O:11]C)=[O:10])=[O:4].[OH-].[Na+]>>[CH3:1][N:2]([CH3:22])[C:3]([S:5][C:6]1[CH:7]=[C:8]([CH:13]=[C:14]([S:16][C:17](=[O:21])[N:18]([CH3:20])[CH3:19])[CH:15]=1)[C:9]([OH:11])=[O:10])=[O:4]

Komponenten

3

Edukt 2

HCID 14798Sodium HydroxideHCID 12138342Methyl 3,5-bis(dimethylcarbamoylthio)benzoate

Produkt 1

HCID 12138351HCID 12138351, VerbindungAusbeute 87,2 %

Versuchsvorschrift

Methyl 3,5-bis(dimethylcarbamoylthio)benzoate (3.42 g, 10 mmol) was made to react with 5% aqueous sodium hydroxide solution (10 ml. 12.5 mmol) for 3 hours at 22–25° C. with stirring. After cooling by the addition of 50 ml of ice-water, the reaction mixture was extracted with ethyl acetate (300 ml×3) and the extract was dried over magnesium sulfate. The ethyl acetate was evaporated under reduced pressure and the colorless crystals thus obtained was recrystallized from ethanol to give 2.86 g (87.2%) of 3,5-bis(dimethylcarbamoylthio)benzoic acid as colorless needles. The melting point is 196–198° C. (with decomposition).

Aufarbeitung

  1. extractionthe reaction mixture was extracted with ethyl acetate (300 ml×3)
  2. dry with materialthe extract was dried over magnesium sulfate
  3. customThe ethyl acetate was evaporated under reduced pressure
  4. customthe colorless crystals thus obtained
  5. customwas recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-f664399a9bc0413e9379e3c931517d37
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07205428B2

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