Dimethylformamide → HCID 18383995, Verbindung

HRID 2297731Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2297731
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([OH:11])[C:9]=1[OH:10])[CH:5]=[O:6].[C:12](=[O:15])([O-])[O-].[K+].[K+].[CH3:18][O:19][CH2:20]Cl.[CH3:22]N(C)C=O>>[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([O:11][CH2:22][O:15][CH3:12])[C:9]=1[O:10][CH2:18][O:19][CH3:20])[CH:5]=[O:6]

Komponenten

5

Edukt 4

HCID 6228DimethylformamideHCID 7864Chloromethyl Methyl EtherHCID 11430Potassium CarbonateHCID 836513,4,5-Trihydroxybenzaldehyde

Produkt 1

HCID 18383995HCID 18383995, VerbindungAusbeute 17 %

Versuchsvorschrift

3,4,5-Trihydroxybenzaldehyde (628 mg, 3.6 mmol) was dissolved in dimethylformamide (30 mL), and potassium carbonate (2.0 g, 14 mmol) was added thereto, followed by stirring at room temperature for 30 minutes. Next, chloromethyl methyl ether (0.96 mL, 13 mmol) was added thereto, followed by stirring at room temperature for 2 hours. After the conventional post-treatment, the residue was purified by preparative thin layer chromatography (developed with chloroform/methanol=98/2) to give 3-hydroxy-4,5-bis(methoxymethoxy)benzaldehyde (140 mg, yield 17%).

Aufarbeitung

  1. stirringby stirring at room temperature for 2 hours
  2. customAfter the conventional post-treatment, the residue was purified by preparative thin layer chromatography (developed with chloroform/methanol=98/2)

Quellen und Nachweise

ORD-Eintrag
ord-21707e02c84548ddb23ab068bf97fe96
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06492392B1

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