HCID 178482203, Verbindung → HCID 178482196, Verbindung

HRID 485753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 485753
[CH3:1][NH:2][C:3]1[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][C:4]=1[C:5]([N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([OH:16])=[N:8]1)=[O:6]>CCO.[Pd]>[CH3:1][NH:2][C:3]1[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][C:4]=1[C:5]([N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([OH:16])=[N:8]1)=[O:6]

Komponenten

4

Edukt 1

HCID 178482203HCID 178482203, Verbindung

Produkt 1

HCID 178482196HCID 178482196, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

To 1.1 g. of 1-(2-methylamino-5-nitrobenzoyl)-1H-indazol-3-ol, prepared in Example 14, suspended in 200 ml of absolute EtOH was added 200 mg of 5% Pd/C and the mixture was hydrogenated at 50 psi for 16 hours. The catalyst was filtered off, washed with hot EtOH and the filtrate was diluted with H2O and concentrated to small volume. The precipitate was collected, washed with cold 95% EtOH and dried; yield of dark-yellow amorphous powder 0.65 g. (65.4%); m.p. 184°-186° C.

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. washwashed with hot EtOH
  3. additionthe filtrate was diluted with H2O
  4. concentrationconcentrated to small volume
  5. customThe precipitate was collected
  6. washwashed with cold 95% EtOH
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2e1ea073a0d54675ae6a193630976836
Quelldatensatz
uspto-grants-1985_08
Patentnummer
US04537966

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