Formaldehyde → HCID 69433836, Verbindung

HRID 1294453Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1294453
Cl.[C:2]([C:4]1[CH:12]=[CH:11][C:7]([CH2:8][O:9][NH2:10])=[C:6]([O:13][CH2:14][CH3:15])[CH:5]=1)#[N:3].[CH3:16][OH:17].C=O>O>[C:2]([C:4]1[CH:12]=[CH:11][C:7]([CH2:8][O:9][NH2:10])=[C:6]([O:13][CH2:14][CH3:15])[CH:5]=1)#[N:3].[CH2:16]=[O:17]

Komponenten

5

Edukt 3

HCID 712FormaldehydeHCID 887MethanolHCID 69434226O-(4-cyano-2-ethoxybenzyl)hydroxyamine hydrochloride

Produkt 1

HCID 69433836HCID 69433836, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

O-(4-cyano-2-ethoxybenzyl)hydroxyamine hydrochloride (19-1, 2.7 g, 0.012 mol), methanol (20 ml) and water (20 ml) were charged, and a 36% formaldehyde aqueous solution was added to this, and the mixture was stirred at room temperature for 2.0 hours. Water was added to the mixture and the mixture was extracted with ethyl acetate. The resulted ethyl acetate layer was dried over anhydrous magnesium sulfate, then, the solvent was distilled off under reduce pressure. This was purified by silica gel column chromatography using hexane/ethyl acetate system, to obtain O-(4-cyano-2-ethoxybenzyl)hydroxyamine-formaldehyde derivative (3-1a, 2.2 g, yield 96%).

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe resulted ethyl acetate layer was dried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off
  4. customThis was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-b635086fdb4b4c5d979b53b05dc73ddb
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07241625B2

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