Phosgene → (2-Chloroethyl)phosphonic dichloride

HRID 464571

반응식

HRID 464571 반응식
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]

참가 물질

6

반응물 3

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

생성물 2

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

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-25d1c16c6c294e8e9cbd790bf3c62f03
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04548762

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