HCID 22013736, Verbindung → HCID 22013776, Verbindung

HRID 1532690Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1532690
[CH3:1][N:2]([CH3:19])[CH2:3][CH2:4][NH:5][C:6]1[CH:15]=[CH:14][C:9]([C:10]([NH:12][CH3:13])=[O:11])=[CH:8][C:7]=1[N+:16]([O-])=O>C(OCC)(=O)C.C(O)C.[C].[Pd]>[NH2:16][C:7]1[CH:8]=[C:9]([CH:14]=[CH:15][C:6]=1[NH:5][CH2:4][CH2:3][N:2]([CH3:1])[CH3:19])[C:10]([NH:12][CH3:13])=[O:11]

Komponenten

5

Edukt 1

HCID 22013736HCID 22013736, Verbindung

Produkt 1

HCID 22013776HCID 22013776, VerbindungAusbeute 87,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

10% of palladium-carbon (0.738 g) was added to a solution containing 4-{[2-(dimethylamino)ethyl]amino}-N-methyl-3-nitrobenzamide (3.679 g) in a mixture of ethyl acetate (40 ml) and ethanol (37 ml), and the mixture was stirred for 4.5 hours under a hydrogen gas atmosphere at room temperature. After the catalyst was removed out by filtration, the filtrate was concentrated. The residue, with ethyl acetate added thereto, was washed with 1N sodium hydroxide aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and concentrated, thereby yielding the entitled compound (2.862 g) as brown solid.

Aufarbeitung

  1. customAfter the catalyst was removed out by filtration
  2. concentrationthe filtrate was concentrated
  3. additionThe residue, with ethyl acetate added
  4. washwas washed with 1N sodium hydroxide aqueous solution and saturated brine successively
  5. dry with materialdried over sodium sulfate anhydride
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-266c1b073c7041498535b829c453d6cb
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06204264B1

Notizen zur Reaktion

Wird geladen…