9-Oxofluorene-4-carboxylic acid → HCID 59208194, Verbindung

HRID 2243314

Reaktionsgleichung

Reaktionsgleichung von HRID 2243314
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH-:8].[O:9]=[C:10]1[C:22]2[CH:21]=[CH:20][CH:19]=[C:18]([C:23](O)=O)[C:17]=2[C:16]2[C:11]1=[CH:12][CH:13]=[CH:14][CH:15]=2>C(O)(=O)C>[NH:1]1[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[N:8]=[C:23]1[C:18]1[C:17]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=[O:9])[C:22]=2[CH:21]=[CH:20][CH:19]=1

Komponenten

4

Edukt 2

HCID 803619-Oxofluorene-4-carboxylic acidHCID 86621027HCID 86621027, Verbindung

Produkt 1

HCID 59208194HCID 59208194, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

In a 50-ml three-necked flask under an argon atmosphere, heat, at 80° C. for 2 hours, a solution of 3 g of the (2-amino-phenyl)amide of 9-oxo-9H-fluorene-4-carboxylic acid obtained in the preceding stage, in 150 ml of acetic acid. After cooling, the precipitate that formed is drained. After purification by silica gel flash chromatography, eluting with mixtures of dichloromethane and ethyl acetate (90-10 then 80-20 and finally 70-30 by volume), we obtain 1.73 g of 4-(1H-benzimidazol-2-yl)-fluoren-9-one in the form of a yellow powder, which is used as it is in the next stage, with the following characteristics:

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe precipitate that formed
  3. customAfter purification by silica gel flash chromatography
  4. washeluting with mixtures of dichloromethane and ethyl acetate (90-10

Quellen und Nachweise

ORD-Eintrag
ord-91000b449a9f4adba18f981a768e6866
Quelldatensatz
uspto-grants-2010_03
Patentnummer
US07674795B2

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