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Ethyl Acetate → HCID 90308710, Verbindung

HRID 2283692
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2283692
C(OCC)(=O)C.[CH3:7][N:8]1[CH:16]=[C:15]2[C:10]([C:11]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:12][C:13]([N+:17]([O-])=O)=[CH:14]2)=[N:9]1>[Pd].C1COCC1>[CH3:7][N:8]1[CH:16]=[C:15]2[C:10]([C:11]([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)=[CH:12][C:13]([NH2:17])=[CH:14]2)=[N:9]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 8857Ethyl AcetateHCID 90308830HCID 90308830, Verbindung

Produkt 1

HCID 90308710HCID 90308710, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Ethyl acetate (5 mL) and THF (2 mL) were added to 2-methyl-5-nitro-7-phenyl-2H-indazole obtained in the above-described Step 2 (260 mg). Thereafter, 10% palladium on carbon (300 mg) was added under nitrogen atmosphere, and the reaction solution was stirred under hydrogen atmosphere at room temperature overnight. The insolubles were filtrated, and then the solvent was evaporated under vacuum. Subsequently, the resultant residue was purified by column chromatography on basic silica gel (developing solvent:hexane/ethyl acetate) to obtain 2-methyl-7-phenyl-2H-indazol-5-amine as brown amorphous.

Aufarbeitung

  1. customobtained in the above-described Step 2 (260 mg)
  2. filtrationThe insolubles were filtrated
  3. customthe solvent was evaporated under vacuum
  4. customSubsequently, the resultant residue was purified by column chromatography on basic silica gel (developing solvent:hexane/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-c4cb943ba6dc436da8e776c23f5515e3
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09145414B2

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