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

HRID 1975543노트

반응식

HRID 1975543 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a702c35e5151447aac5eba41099f7a81
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05286905

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