HCID 21468845, Verbindung → HCID 178442273, Verbindung

HRID 1938630Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1938630
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=2[C:11]#[N:12])[CH:5]=[CH:6][C:7]=1[NH2:8]>C(O)C>[C:11]([C:10]1[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=1[C:4]1[CH:5]=[CH:6][C:7]2[NH:8][C:4]([CH2:3][CH2:2][CH2:7][CH2:6][CH3:5])=[N:1][C:2]=2[CH:3]=1)#[N:12]

Komponenten

3

Edukt 1

HCID 21468845HCID 21468845, Verbindung

Produkt 1

HCID 178442273HCID 178442273, VerbindungAusbeute 160,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

2-(3,4-Diaminophenyl)benzonitrile (4.3 mmoles, 0.9 g) and ethyl hexanoamidate hydrochloride were dissolved in 20 ml ethanol and stirred for 2.5 hours. The solvent was removed in vacuo. The residue was dissolved in ethyl acetate and washed with water, saturated NaHCO3 and brine. The organic phase was dried and concentrated. The residue was chromatographed on silica gel eluted with 1: ethylacetate/hexane to yield 1.0 g of 5-(2-Cyanophenyl)-2-pentyl-1H-benzimidazole.

Aufarbeitung

  1. customThe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with water, saturated NaHCO3 and brine
  4. customThe organic phase was dried
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel
  7. washeluted with 1

Quellen und Nachweise

ORD-Eintrag
ord-b273ebee56c649bf959eab472e8cd812
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05693633

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