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Water → 2-(3-Methylbutyl)aniline

HRID 1359941
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HRID 1359941 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=O)[CH2:9][CH:10]([CH3:12])[CH3:11].O.NN.[OH-].[K+].O>C(O)COCCOCCO.C(OCC)(=O)C>[CH3:11][CH:10]([CH3:12])[CH2:9][CH2:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[NH2:1]
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참가 물질

7

반응물 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 122976091-(2-Aminophenyl)-3-methylbutan-1-one

생성물 1

HCID 187640942-(3-Methylbutyl)aniline수율 72.1%

시약·촉매·용매 2

HCID 8172Triethylene Glycol용매
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HCID 8857
Ethyl Acetate
용매

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온도
210 °C

실험 절차

A solution comprising 8.0 g (0.045 mol) of 1-(2-aminophenyl)-3-methylbutan-1-one (X-1), 6.8 g (0.135 mol) of hydrazine hydrate and 7.6 g (0.135 mol) of potassium hydroxide in 90 ml of triethylene glycol is heated at 210° C. for 6 h. For work-up, water and ethyl acetate are added at room temperature. The organic phase is again washed with water, dried over magnesium sulphate and concentrated under reduced pressure. Purification by column chromatography (cyclohexane/ethyl acetate 3:1) gives 5.3 g (71.5% of theory) of [2-(3-methylbutyl)-phenyl]amine.

후처리

  1. washThe organic phase is again washed with water
  2. dry with materialdried over magnesium sulphate
  3. concentrationconcentrated under reduced pressure
  4. customPurification by column chromatography (cyclohexane/ethyl acetate 3:1)

출처 및 근거

ORD 기록
ord-cb8e894fb6f642e68ae41001b4f15a85
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07879760B2

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