Phosgene → (2-Chloroethyl)phosphonic dichloride

HRID 464571

Reaktionsgleichung

Reaktionsgleichung von HRID 464571
C(P(=O)(O)O)=C.[CH:7]([P:9]([Cl:12])([Cl:11])=[O:10])=[CH2:8].[C:13]([Cl:16])(Cl)=O>ClCCCl>[CH:7]([P:9]([Cl:12])([Cl:11])=[O:10])=[CH2:8].[Cl:16][CH2:13][CH2:7][P:9]([Cl:12])([Cl:11])=[O:10]

Komponenten

6

Edukt 3

HCID 6371PhosgeneHCID 74035Phosphonic dichloride, ethenyl-HCID 168725Poly(vinylphosphonic acid)

Produkt 2

HCID 69645(2-Chloroethyl)phosphonic dichlorideHCID 74035Phosphonic dichloride, ethenyl-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

298 g of the vinylphosphonic acid derivatives thus prepared are metered into 300 g of vinylphosphonic acid dichloride at 145° C. during the course of 4 hours, whilst stirring, during which time phosgene gas is continuously introduced into the reaction mixture. The reaction mixture is then further phosgenated for 10 hours at this temperature. 1,2-Dichloroethane which is formed distils off during the phosgenation. After the phosgenation has ended, the excess phosgene is stripped off at room temperature in the vacuum from a water jet. The mixture is then distilled at 2 mm Hg with the aid of a column. 430 g of vinylphosphonic acid dichloride and 140 g of 2-chloroethanephosphonic acid dichloride are obtained. The distillation residue is 39 g. 130 g of vinylphosphonic acid dichloride and 140 g of 2-chloroethanephosphonic acid dichloride were thus prepared from 298 g of vinylphosphonic acid derivatives. The 2-chloroethanephosphonic acid dichloride can again be employed as the reaction medium in a second mixture, instead of the vinylphosphonic acid dichloride.

Aufarbeitung

  1. additionis continuously introduced into the reaction mixture
  2. customdistils off during the phosgenation
  3. customis stripped off at room temperature in the vacuum from a water jet
  4. distillationThe mixture is then distilled at 2 mm Hg with the aid of a column

Quellen und Nachweise

ORD-Eintrag
ord-25d1c16c6c294e8e9cbd790bf3c62f03
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04548762

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