Ethyl Acetoacetate → HCID 22387816, Verbindung

HRID 1072779Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1072779
[N+](C1C=C([N+]([O-])=O)C=CC=1O)([O-])=O.[NH2:14][N:15]1[CH:25]=[CH:24][C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:17][CH2:16]1.C(=O)([O-])[O-].[K+].[K+].[C:32]([O:38][CH2:39][CH3:40])(=[O:37])[CH2:33][C:34]([CH3:36])=O>C(O)C>[CH3:36][C:34]1[C:33]([C:32]([O:38][CH2:39][CH3:40])=[O:37])=[C:25]2[CH:24]=[C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:17]=[CH:16][N:15]2[N:14]=1

Komponenten

5

Edukt 3

HCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 22388182HCID 22388182, Verbindung

Produkt 1

HCID 22387816HCID 22387816, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Ethyl N-aminoisonicotinate 2,4-dinitrophenol salt (10.2 g) was suspended in ethanol (147 ml), and potassium carbonate (3.77 g) was added, which was followed by stirring at room temperature for 30 min. To the mixture was added ethyl acetoacetate (3.69 ml), and the mixture was stirred at 60° C. for 5 hr with heating. The insoluble matter was filtered off and the filtrate was concentrated to dryness under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=7/1) to give the objective compound (2.70 g) as an amber-colored solid.

Aufarbeitung

  1. stirringthe mixture was stirred at 60° C. for 5 hr
  2. temperaturewith heating
  3. filtrationThe insoluble matter was filtered off
  4. concentrationthe filtrate was concentrated to dryness under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=7/1)

Quellen und Nachweise

ORD-Eintrag
ord-00ec18c89f014e61be3b942ae398d67b
Quelldatensatz
uspto-grants-2005_06
Patentnummer
US06911469B2

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