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Sulfuric Acid → 3-[Ethyl(hydroxy)phosphoryl]propanoic acid

HRID 1028258
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반응식

HRID 1028258 반응식
[Na+].[CH2:2]([P:4]([OH:11])([CH2:6][CH2:7][C:8]([O-:10])=[O:9])=[O:5])[CH3:3].S(=O)(=O)(O)O>O>[CH2:2]([P:4]([OH:11])([CH2:6][CH2:7][C:8]([OH:10])=[O:9])=[O:5])[CH3:3]
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참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 1317314203-(Ethylhydroxyphosphinyl)propionic acid sodium salt

생성물 1

HCID 190110643-[Ethyl(hydroxy)phosphoryl]propanoic acid수율 98%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

630 g (3 mol) of 3-(ethylhydroxyphosphinyl)propionic acid sodium salt (produced as in Example 16) are dissolved in 860 g of water and initially charged into a 5 l five-neck flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel and neutralized by addition of about 147 g (1.5 mol) of concentrated sulfuric acid. The water is subsequently distilled off in vacuo. The residue is taken up in ethanol and the insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo to leave 488 g (98% of theory) of 3-(ethylhydroxy-phosphinyl)propionic acid as a solid material.

후처리

  1. additioninitially charged into a 5 l five-neck flask
  2. customequipped with thermometer
  3. temperaturereflux condenser, high-performance stirrer
  4. distillationThe water is subsequently 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-e8275dfa450d4b34a6186bb1fe055b14
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735477B2

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