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Hydrogen Peroxide → Tetradecyldimethylamine oxide dihydrate

HRID 344976
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HRID 344976 반응식
[CH2:1]([N:15]([CH3:17])[CH3:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].C(N(CC(O)=O)CCN(CC(O)=O)CC(O)=O)CN(CC(O)=O)CC(O)=[O:23].[OH:45]O>C(OCC)(=O)C>[OH2:23].[OH2:45].[CH2:1]([N+:15]([O-:23])([CH3:17])[CH3:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]
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참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 3053Diethylenetriaminepentaacetic acidHCID 8211N,N-Dimethyltetradecylamine

생성물 1

HCID 21983433Tetradecyldimethylamine oxide dihydrate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

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온도
65 °C

실험 절차

In a 250 milliliter glass reaction flask was placed 100 grams of tetradecyldimethylamine (0.41 mole; amine value 230.0 mg KOH/g amine) and 0.5 gram (1.27 mmol) of diethylenetriaminepentaacetic acid. This was heated with stirring to 65° C. and then 23 grams (0.47 mole) of 70 weight percent aqueous hydrogen peroxide was added dropwise over a 15-minute period. The mixture was then heated to 76° C. and stirred at that temperature for seven hours. As needed, ethyl acetate (34 mL) was added dropwise to the reaction mass in order to maintain a clear, gel-free liquid. Analysis of the crude reaction mass showed 99 percent amine conversion by proton NMR. The crude reaction mass was added to 400 mL additional ethyl acetate. The solution was then cooled to 15° C. forming a non-hydroscopic white crystalline solid tetradecyldimethylamine oxide dihydrate in 86% recovered yield melting at about 41° C.

후처리

  1. temperatureThis was heated
  2. temperatureThe mixture was then heated to 76° C.
  3. stirringstirred at that temperature for seven hours
  4. temperatureto maintain a clear, gel-free liquid
  5. customAnalysis of the crude reaction mass
  6. customThe crude reaction mass
  7. temperatureThe solution was then cooled to 15° C.

출처 및 근거

ORD 기록
ord-7144b3b5aef5448aa3ea3d6c58be61c5
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05055233

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