3,4-Dimethylaniline → N-(1-ethylpropyl)-3,4-dimethylaniline

HRID 443777노트

반응식

HRID 443777 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([CH3:9])[CH:3]=1.[CH2:10]([C:12]([CH2:14][CH3:15])=O)[CH3:11]>[Pt].C(O)(=O)C>[CH3:11][CH2:10][CH:12]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([CH3:9])[CH:3]=1)[CH2:14][CH3:15]

참가 물질

5

반응물 2

HCID 72483,4-DimethylanilineHCID 7288Ethyl ketone

생성물 1

HCID 91984N-(1-ethylpropyl)-3,4-dimethylaniline수율 72.2%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 176Acetic Acid용매

반응 조건

온도
60 °C

실험 절차

Amounts of 24.2 g (0.20 mole) of 3,4-xylidine 38.4 g (0.44 mole) of diethyl ketone, 1.2 g of 5% platinum on carbon, and 0.26 g (2 mole %) of glacial acetic acid were charged to an autoclave and the autoclave was sealed, evacuated, purged with hydrogen and then pressurized with hydrogen to 50 psi. The temperature of the autoclave was raised to 60° C. and held at 60°-68° C. for 0.9 hours (very little, if any, hydrogen was being absorbed at this point). The autoclave was vented and the product filtered to separate the catalyst. The lower, aqueous phase, of the filtrate was separated and the upper, organic phase, was evaporated to constant weight of 35.0 g. Analysis of the residue showed it to be 78.8% pure, corresponding to 28.7 g of N-3-pentyl-3,4-xylidine (72.2% yield).

후처리

  1. customthe autoclave was sealed
  2. customevacuated
  3. custompurged with hydrogen
  4. custom(very little, if any, hydrogen was being absorbed at this point)
  5. filtrationthe product filtered
  6. customto separate the catalyst
  7. customThe lower, aqueous phase, of the filtrate was separated
  8. customthe upper, organic phase, was evaporated to constant weight of 35.0 g

출처 및 근거

ORD 기록
ord-51a3a87a9dbf4db8800e4981c1101536
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04261926

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