Ethanol → HCID 178423444, Verbindung

HRID 916082Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 916082
[C:1]1([CH2:11][NH:12][C:13]2[CH:18]=C[C:16](C)=[CH:15][C:14]=2[NH2:20])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[SH-:21].[C+4:22].[SH-].[SH-].[SH-].[CH2:26](O)[CH3:27]>>[C:1]1([CH2:11][N:12]2[C:13]3[CH:18]=[C:26]([CH3:27])[CH:16]=[CH:15][C:14]=3[N:20]=[C:22]2[SH:21])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 3

HCID 702EthanolHCID 17810729((1-Naphthyl)methyl)(2-amino-4-methyl-phenyl)amineHCID 178420937HCID 178420937, Verbindung

Produkt 1

HCID 178423444HCID 178423444, VerbindungAusbeute 44 %

Versuchsvorschrift

Subsequently, ((1-naphthyl)methyl)(2-amino-4-methyl-phenyl)amine (943.1 mg, 3.59 mmol) was dissolved in ethanol (6.4 ml), to which carbon bisulfide (7 ml, 116 mmol) was added, and then refluxed. After 10 hours, it was returned to room temperature, concentrated under reduced pressure. Ethanol (2 ml) was added to the residue, which was stirred at room temperature for 30 minutes, and was further stirred on ice for 30 minutes. The resulting crystals were filtered, and dried to obtain 1-((1-naphthyl)methyl)-6-methyl-benzimidazole-2-thiol (459.1 mg, yield 44%, 2 steps).

Aufarbeitung

  1. additionwas added
  2. temperaturerefluxed
  3. customwas returned to room temperature
  4. concentrationconcentrated under reduced pressure
  5. additionEthanol (2 ml) was added to the residue, which
  6. stirringwas further stirred on ice for 30 minutes
  7. filtrationThe resulting crystals were filtered
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-24e62a9e4c214738bfaf1dc9e2a399eb
Quelldatensatz
uspto-grants-2007_09
Patentnummer
US07268145B2

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