Hydrochloric Acid → HCID 178473964, Verbindung

HRID 1637954

Reaktionsgleichung

Reaktionsgleichung von HRID 1637954
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([N+:13]([O-:15])=[O:14])=[CH:10][CH:11]=2)[CH2:6][C:5]1=[O:16])(=[O:3])[CH3:2].[F:17][C:18]([F:29])([F:28])[C:19]1[CH:27]=[CH:26][C:22]([C:23](O)=[O:24])=[CH:21][CH:20]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C1C=CC2N(O)N=NC=2C=1.Cl>CN(C=O)C>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([N+:13]([O-:15])=[O:14])=[CH:10][CH:11]=2)[C:6](=[C:23]([OH:24])[C:22]2[CH:26]=[CH:27][C:19]([C:18]([F:17])([F:28])[F:29])=[CH:20][CH:21]=2)[C:5]1=[O:16])(=[O:3])[CH3:2]

Komponenten

7

Edukt 5

HCID 313Hydrochloric AcidHCID 99664-(Trifluoromethyl)benzoic acidHCID 757711-HydroxybenzotriazoleHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 28393291-Acetyl-5-nitroindolin-2-one

Produkt 1

HCID 178473964HCID 178473964, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Prepared by reacting 1-acetyl-5-nitro-2-indolinone with one equivalent of 4-trifluoromethyl-benzoic acid in dry DMF in the presence of 1 equivalent each of TBTU and HOBT and 5 equivalents of Huinig's base (20° C., 4 hours), stirring into dilute hydrochloric acid, filtering the precipitate, dissolving the precipitate in EtOac, drying the organic phase and evaporation in vacuo and purifying the evaporation residue by column chromatography on silica gel with CH2Cl2 /MeOH (10:1) as eluant.

Aufarbeitung

  1. customPrepared
  2. filtrationfiltering the precipitate
  3. dissolutiondissolving the precipitate in EtOac
  4. customdrying
  5. customthe organic phase and evaporation in vacuo
  6. custompurifying the evaporation residue by column chromatography on silica gel with CH2Cl2 /MeOH (10:1) as eluant

Quellen und Nachweise

ORD-Eintrag
ord-ced276462a764a7a8b4fce8abba231b5
Quelldatensatz
uspto-grants-2000_03
Patentnummer
US06043254

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