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Methane → [Hydroxy(ethyl)phosphinyl]acetic acid

HRID 1526927
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1526927
[CH2:1]([P:3]([CH2:6][CH2:7][OH:8])(=[O:5])[OH:4])[CH3:2].[OH-:9].[Na+].C>O>[CH2:1]([P:3]([OH:4])([CH2:6][C:7]([OH:9])=[O:8])=[O:5])[CH3:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 297MethaneHCID 14798Sodium Hydroxide2×HCID 46832563HCID 46832563, Verbindung

Produkt 1

HCID 15357685[Hydroxy(ethyl)phosphinyl]acetic acidAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

13.8 g (0.1 mol) of ethyl(2-hydroxyethyl)phosphinic acid (produced as in Example 7) are dissolved in 150 ml of water and adjusted to pH 9 with 2N NaOH solution. Then, 0.45 g of charcoal with 5% Pt and 1% Bi is added, the suspension is heated to 70° C. and air is passed through the suspension at a rate of 10 l/h. All the while, the pH of the suspension is maintained at pH=9 by adding 2N NaOH solution. After the reaction has ended, the reaction solution is filtered to remove the catalyst, which is washed, the filtrate is made acidic with hydrochloric acid and the water is distilled off in vacuo. The residue is taken up in tetrahydrofuran and extracted. The insoluble salts are filtered off to leave 14.0 g (92% of theory) of 2-(ethylhydroxyphosphinyl)acetic acid as colorless solid.

Aufarbeitung

  1. temperatureAll the while, the pH of the suspension is maintained at pH=9
  2. filtrationthe reaction solution is filtered
  3. customto remove the catalyst, which
  4. washis washed
  5. distillationthe water is distilled off in vacuo
  6. extractionextracted
  7. filtrationThe insoluble salts are filtered off

Quellen und Nachweise

ORD-Eintrag
ord-452e082171bf4e4489dcdfc7a20a4e5d
Quelldatensatz
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09085734B2

Notizen zur Reaktion

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