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

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>>[CH2:2]([P:4]([OH:11])([CH2:6][CH2:7][C:8]([OH:10])=[O:9])=[O:5])[CH3:3]

참가 물질

반응물 2

HCID 1118Sulfuric Acid

HCID 1317314203-(Ethylhydroxyphosphinyl)propionic acid sodium salt

생성물 1

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

실험 절차

In the aqueous solution of 420 g (2 mol) of 3-(ethylhydroxyphosphinyl)propionic acid sodium salt (produced as in Example 12) is rendered acidic with about 196 g of concentrated sulfuric acid and the water is distilled off in vacuo. The residue was taken up in tetrahydrofuran and extracted. The insoluble salts were filtered off. The solvent of the filtrate was removed in vacuo and the residue was recrystallized from acetone to obtain 325 g (98% of theory) of 3-(ethylhydroxyphosphinyl)-propionic acid as colorless solid.

후처리

distillationthe water is distilled off in vacuo
extractionextracted
filtrationThe insoluble salts were filtered off
customThe solvent of the filtrate was removed in vacuo
customthe residue was recrystallized from acetone

출처 및 근거

ORD 기록: ord-1e84d5a3e98a470ca21dece40bd98be2
출처 데이터셋: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09139714B2

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