9-Oxofluorene-4-carboxylic acid → HCID 67359009, Verbindung

HRID 2243324

Reaktionsgleichung

Reaktionsgleichung von HRID 2243324
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH-:9].[O:10]=[C:11]1[C:23]2[CH:22]=[CH:21][CH:20]=[C:19]([C:24](O)=O)[C:18]=2[C:17]2[C:12]1=[CH:13][CH:14]=[CH:15][CH:16]=2.C(=O)([O-])O.[Na+]>C(O)(=O)C.O>[CH3:8][C:4]1[C:3]2[N:9]=[C:24]([C:19]3[C:18]4[C:17]5[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=5)[C:11](=[O:10])[C:23]=4[CH:22]=[CH:21][CH:20]=3)[NH:1][C:2]=2[CH:7]=[CH:6][CH:5]=1

Komponenten

6

Edukt 3

HCID 803619-Oxofluorene-4-carboxylic acidHCID 516892Sodium BicarbonateHCID 86621029HCID 86621029, Verbindung

Produkt 1

HCID 67359009HCID 67359009, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

The procedure used in Example 68 is followed. In a 250 ml round-bottomed flask under an argon atmosphere, reflux, for 6 hours, a suspension of 5 g of (2-amino-6-methylphenyl)amide of 9-oxo-9H-fluorene-4-carboxylic acid, obtained in the previous stage, in 100 ml of acetic acid. After cooling, bring to dryness under reduced pressure. Take the residue up in 25 ml of water then bring to pH=8 by addition of a saturated aqueous solution of sodium hydrogen carbonate. The precipitate that formed is filtered off, washed with water, and made into a paste with diisopropyl ether, and in this way, we obtain 4.7 g of 4-(4-methyl-1H-benzimidazol-2-yl)-9H-fluoren-9-one, in the form of an orange powder, which is used as it is in the following stage, with the following characteristics:

Aufarbeitung

  1. temperatureIn a 250 ml round-bottomed flask under an argon atmosphere, reflux, for 6 hours
  2. temperatureAfter cooling
  3. customThe precipitate that formed
  4. filtrationis filtered off
  5. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-dddcc537beb54a5384c268608f75438e
Quelldatensatz
uspto-grants-2010_03
Patentnummer
US07674795B2

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