Hydroxyamine hydrochloride → 3-Chloro-4-methylbenzaldoxime

HRID 1880232Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1880232
[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-methylbenzaldoxime

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To 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 the resultant mixture was stirred at room temperature for 2 hours. After the completion of the reaction, the reaction mixture was diluted with 70 mL of ethyl acetate and the diluted reaction mixture was washed with water (30 mL×1) and then dehydrated and dried over saturated saline and anhydrous sodium sulfate in this order, followed by distilling off the solvent under reduced pressure to obtain 5.1 g of the objective substance as a white crystal. This crystal was used in the next process as it was without being further purified.

Aufarbeitung

  1. customAfter the completion of the reaction
  2. customthe diluted reaction mixture
  3. washwas washed with water (30 mL×1)
  4. dry with materialdried over saturated saline and anhydrous sodium sulfate in this order
  5. distillationby distilling off the solvent under reduced pressure
  6. customto obtain 5.1 g of the objective substance as a white crystal

Quellen und Nachweise

ORD-Eintrag
ord-a1e18b6c285f4eaca6ba2e6163199e31
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08318757B2

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