Water → HCID 178509651, Verbindung

HRID 976576Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 976576
[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-0b206c4cb23241d09f7958fdf1d6e38a
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05612360

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