1-(3,5-Dimethylphenoxy)-2-propanone oxime → 2-(3,5-Dimethyl-phenoxy)-1-methyl-ethylamine

HRID 1975543Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1975543
[CH3:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12]([CH3:14])[CH:13]=1)[O:5][CH2:6][C:7](=[N:9]O)[CH3:8]>C(O)C.[Ni]>[CH3:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12]([CH3:14])[CH:13]=1)[O:5][CH2:6][CH:7]([NH2:9])[CH3:8]

Komponenten

4

Edukt 1

HCID 731208521-(3,5-Dimethylphenoxy)-2-propanone oxime

Produkt 1

HCID 53052572-(3,5-Dimethyl-phenoxy)-1-methyl-ethylamineAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

10.0 Grams (52 mmol) of 1-(3,5-dimethylphenoxy)-2-propanone oxime was dissolved in 50 ml of ethanol in an autoclave, and 1.0 g of a Raney nickel catalyst (W-2) was added. The resultant mixture was stirred under a hydrogen pressure of 5 kg/cm2G at 50° to 60° C. for 1 hour. The catalyst was separated by filtration, and the filtrate was concentrated under reduced pressure. The residue was dissolved in 50 ml of ethyl ether, and the mixture was subjected to extraction with a 20% hydrochloric acid aqueous solution. The extracted water layer was made alkaline with a 20% sodium hydroxide aqueous solution, and subjected to extraction with 50 ml of ethyl ether. The extracted organic layer was distilled under reduced pressure to give 8.01 g (yield 86%) of 1-(3,5-dimethylphenoxy)2-aminopropane (boiling point 113° C./3 mmHg).

Aufarbeitung

  1. additionwas added
  2. customThe catalyst was separated by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in 50 ml of ethyl ether
  5. extractionthe mixture was subjected to extraction with a 20% hydrochloric acid aqueous solution
  6. extractionsubjected to extraction with 50 ml of ethyl ether
  7. distillationThe extracted organic layer was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a702c35e5151447aac5eba41099f7a81
Quelldatensatz
uspto-grants-1994_02
Patentnummer
US05286905

Notizen zur Reaktion

Wird geladen…