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Vinyl Acetate → Ethyl(2-acetoxyethyl)phosphinic acid

HRID 1028261
ノート
印刷プレビュー

反応式

HRID 1028261 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7904Vinyl AcetateHCID 62655Sodium PersulfateHCID 13411864Ethylphosphonous acid

生成物 1

HCID 46235412Ethyl(2-acetoxyethyl)phosphinic acid収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a00a39ae7eb34a309dc8c78877c0df8b
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735476B2

反応ノート

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