Dimethylformamide → HCID 54001055, Verbindung

HRID 128911Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 128911
C(=O)([O-])[O-].[K+].[K+].[CH2:7](Cl)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.CN(C=O)C.[Cl:20][C:21]1[CH:42]=[CH:41][C:24]([CH2:25][O:26][C:27]2[CH:40]=[CH:39][CH:38]=[CH:37][C:28]=2[C:29]([N:32]2[CH:36]=[CH:35][N:34]=[CH:33]2)=[N:30][OH:31])=[CH:23][CH:22]=1>CCOCC>[CH2:7]([O:31][N:30]=[C:29]([N:32]1[CH:36]=[CH:35][N:34]=[CH:33]1)[C:28]1[CH:37]=[CH:38][CH:39]=[CH:40][C:27]=1[O:26][CH2:25][C:24]1[CH:41]=[CH:42][C:21]([Cl:20])=[CH:22][CH:23]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 74003411HCID 74003411, Verbindung

Produkt 1

HCID 54001055HCID 54001055, VerbindungAusbeute 90,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Potassium carbonate (0.21 g), benzyl chloride (0.15 g) and DMF (2 ml) were added to 2-(4-chlorobenzyloxy)-α-(1-imidazolyl)benzaldehyde oxime (0.33 g), and the mixture was stirred at 60° C. for 2 hours. After completion of the reaction, ether (100 ml) was added, and the mixture was extracted with brine (80 ml) twice, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting crude product was purified by silica gel chromatography to give 2-(4-chlorobenzyloxy)-α-(1-imidazolyl)benzaldehyde O-benzyloxime (0.38 g) as colorless crystals. mp. 94°-95.5° C.

Aufarbeitung

  1. additionwas added
  2. extractionthe mixture was extracted with brine (80 ml) twice
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting crude product was purified by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-58973653597b43008ef4d8ed7741f6e7
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05466661

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