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Ethyl vinyl ether → Ethyl(2-ethoxyethyl)phosphinic acid

HRID 878922
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반응식

HRID 878922 반응식
[CH2:1]([P:3]([OH:5])[OH:4])[CH3:2].[CH2:6]([O:8][CH:9]=[CH2:10])[CH3:7].[O-]S(OOS([O-])(=O)=O)(=O)=O.[Na+].[Na+]>O>[CH2:1]([P:3]([CH2:7][CH2:6][O:8][CH2:9][CH3:10])(=[O:5])[OH:4])[CH3:2]
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참가 물질

5

반응물 3

HCID 8023Ethyl vinyl etherHCID 62655Sodium PersulfateHCID 13411864Ethylphosphonous acid

생성물 1

HCID 46235414Ethyl(2-ethoxyethyl)phosphinic acid수율 95.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

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., 504 g (7 mol) of vinyl ethyl ether and 500 g of a 5% strength sodium peroxodisulfate solution (1.5 mol % based on vinyl ethyl ether) 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 953 g (82% of theory) of ethyl(2-ethoxyethyl)phosphinic acid being obtained as 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-7281be16ebb2489c929bf77ac5a1b783
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987489B2

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