Reaction equation
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]Participants
Procedure
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.
Workup
- additionis continuously introduced into the reaction mixture
- customdistils off during the phosgenation
- customis stripped off at room temperature in the vacuum from a water jet
- distillationThe mixture is then distilled at 2 mm Hg with the aid of a column
Sources & evidence
- ORD record
- ord-25d1c16c6c294e8e9cbd790bf3c62f03
- Source dataset
- uspto-grants-1985_10
- Patent number
- US04548762
Linked notes
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