Allyl Alcohol → Ethyl-3-hydroxypropylphosphinic acid

HRID 1914964노트

반응식

HRID 1914964 반응식
[CH2:1]([P:3]([OH:5])[OH:4])[CH3:2].[CH2:6]([OH:9])[CH:7]=[CH2:8].[O-]S(OOS([O-])(=O)=O)(=O)=O.[Na+].[Na+]>O>[CH2:1]([P:3]([CH2:8][CH2:7][CH2:6][OH:9])(=[O:5])[OH:4])[CH3:2]

참가 물질

5

반응물 3

HCID 7858Allyl AlcoholHCID 62655Sodium PersulfateHCID 13411864Ethylphosphonous acid

생성물 1

HCID 86656674Ethyl-3-hydroxypropylphosphinic acid수율 89%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

564 g (6 mol) of ethylphosphonous acid (produced as in Example 1) 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. The reaction mixture is heated to 100° C. and 406 g (7 mol) of allyl alcohol and 500 g of a 5% sodium peroxodisulfate solution (1.5 mol % based on allyl alcohol) is added dropwise at atmospheric pressure over 1 h. Then, the water is distilled off in vacuo, and the residue is taken up in tetrahydrofuran and the insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo to leave 812 g (89% of theory) of ethyl(3-hydroxypropyl)phosphinic acid as oil.

후처리

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

출처 및 근거

ORD 기록
ord-ecff7705adbe4157a25b5afb2e80593f
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614267B2

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