Ethanol → HCID 178488032, Verbindung

HRID 273756

Reaktionsgleichung

Reaktionsgleichung von HRID 273756
C(O)C.[C:4](=[S:6])=S.[NH2:7][C:8]1[CH:9]=[C:10]([O:15][CH3:16])[CH:11]=[CH:12][C:13]=1[NH2:14].[OH-].[Na+]>O>[SH:6][C:4]1[NH:7][C:8]2[CH:9]=[C:10]([O:15][CH3:16])[CH:11]=[CH:12][C:13]=2[N:14]=1

Komponenten

6

Edukt 4

HCID 702EthanolHCID 6348Carbon DisulfideHCID 14798Sodium HydroxideHCID 1534044-Methoxy-o-phenylenediamine

Produkt 1

HCID 178488032HCID 178488032, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

70 ml of ethanol and 15 ml of carbon disulfide were added to 2.6 g of 3,4-diaminoanisole and then a solution of 1.5 g of sodium hydroxide in 5 ml of water was added thereto. After heating with a water bath for 3.5 hours, the mixture was cooled with ice, filtered and then the solvent in the filtrate was distilled off under reduced pressure. The residue was dissolved in ethanol. The solution was filtrated to remove the insoluble matter and then the solvent in the filtrate was distilled off under reduced pressure. The residue was recrystallized from water-containing methanol to obtain 2.0 g of the titled compound (13).

Aufarbeitung

  1. temperatureAfter heating with a water bath for 3.5 hours
  2. temperaturethe mixture was cooled with ice
  3. filtrationfiltered
  4. distillationthe solvent in the filtrate was distilled off under reduced pressure
  5. dissolutionThe residue was dissolved in ethanol
  6. filtrationThe solution was filtrated
  7. customto remove the insoluble matter
  8. distillationthe solvent in the filtrate was distilled off under reduced pressure
  9. customThe residue was recrystallized from water-
  10. additioncontaining methanol

Quellen und Nachweise

ORD-Eintrag
ord-ccbe35180d5349e08245fb39f2fbce2d
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387600

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