Hydroxyamine hydrochloride → 3-Chloro-4-methylbenzaldoxime

HRID 551311Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 551311
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH3:10])[CH:5]=O.Cl.[NH2:12][OH:13]>CO.O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH3:10])[CH:5]=[N:12][OH:13]

Komponenten

6

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 124230853-Chloro-4-methylbenzaldehyde

Produkt 1

HCID 730143123-Chloro-4-methylbenzaldoximeAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

In a solution of 5.0 g of 3-chloro-4-methylbenzaldehyde in 40 mL of methanol and 30 mL of water, 4.7 g of hydroxylamine hydrochloride was added, and stirred at room temperature for 2 hours. After the completion of the reaction, the reaction mixture was diluted with 70 mL of ethyl acetate, washed with water (30 mL×1), and then dehydrated with and dried over saturated sodium chloride and anhydrous sodium sulfate in that order, and the solvent was distilled off under reduced pressure to obtain 5.1 g of the aimed product as white crystal. The resulting product was used as such without purification for the next step.

Aufarbeitung

  1. customAfter the completion of the reaction
  2. washwashed with water (30 mL×1)
  3. dry with materialdried over saturated sodium chloride and anhydrous sodium sulfate in that order
  4. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-19a8d61fd57741d48bda3dd5ec5f07cf
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07947715B2

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