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Vinyl Acetate → Ethyl(2-acetoxyethyl)phosphinic acid

HRID 1028261
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HRID 1028261 반응식
[CH2:1]([P:3]([OH:5])[OH:4])[CH3:2].[C:6]([O:9][CH:10]=[CH2:11])(=[O:8])[CH3:7].[O-]S(OOS([O-])(=O)=O)(=O)=O.[Na+].[Na+]>O>[CH2:1]([P:3]([CH2:11][CH2:10][O:9][C:6](=[O:8])[CH3:7])(=[O:5])[OH:4])[CH3:2]
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참가 물질

5

반응물 3

HCID 7904Vinyl AcetateHCID 62655Sodium PersulfateHCID 13411864Ethylphosphonous acid

생성물 1

HCID 46235412Ethyl(2-acetoxyethyl)phosphinic acid수율 95%

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

564 g (6 mol) of ethylphosphonous acid are dissolved in 860 g of water and initially charged to a 5 l five-neck flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel. After heating the reaction mixture to 100° C., 602 g (7 mol) of vinyl acetate and 500 g of a 5% strength sodium peroxodisulfate solution (1.5 mol % based on vinyl acetate) are added dropwise at atmospheric pressure over 1 h. The water is then distilled off in vacuo. The residue is taken up in tetrahydrofuran and the insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo. Chromatographic purification leaves 1.026 g (95% of theory) of ethyl-(2-acetoxyethyl)phosphinic acid being obtained as an oil.

후처리

  1. additioninitially charged to a 5 l five-neck flask
  2. customequipped with thermometer
  3. temperaturereflux condenser, high-performance stirrer
  4. distillationThe water is then distilled off in vacuo
  5. filtrationthe insoluble salts are filtered off
  6. customThe solvent of the filtrate is removed in vacuo
  7. customChromatographic purification

출처 및 근거

ORD 기록
ord-a00a39ae7eb34a309dc8c78877c0df8b
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735476B2

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