Water → HCID 178509651, Verbindung

HRID 866248Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 866248
[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].O.[F:18][C:19]([F:24])([F:23])[C:20](O)=O>>[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:20]([C:19]([F:24])([F:23])[F:18])=[N:1][C:2]=2[CH:3]=1)#[N:12]

Komponenten

4

Edukt 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 21468845HCID 21468845, Verbindung

Produkt 1

HCID 178509651HCID 178509651, Verbindung

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

2-(3,4-Diaminophenyl)benzonitrile (0.01 moles, 2.09 g) was dissolved in 10 ml trifluoroacetic acid and heated at 85° C. for 16 hours. The solution was poured into water and extracted with ethyl acetate. The pH was adjusted to 3.0 using 5N NaOH. The ethyl acetate was washed with brine, dried over sodium sulfate, and concentrated. The residue was chromatographed on silica gel eluted with 25 % ethyl acetate in hexane. The reaction yielded 2.05 g of 5-(2-cyanophenyl)-2-trifluoromethyl-1H-benzimidazole. (MS)

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate was washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel
  6. washeluted with 25 % ethyl acetate in hexane

Quellen und Nachweise

ORD-Eintrag
ord-5c7d96cc7ffd402cb77dc5ad30d5f663
Quelldatensatz
uspto-grants-1996_10
Patentnummer
US05569768

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