関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Phosphonic dichloride, ethenyl- | HCID 74035 | — |
| 反応物 | Poly(vinylphosphonic acid) | HCID 168725 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | (2-Chloroethyl)phosphonic dichloride | HCID 69645 | — |
| 生成物 | Phosphonic dichloride, ethenyl- | HCID 74035 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04548762 |
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| 出典データセット | uspto-grants-1985_10 |
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| ORD ID | ord-25d1c16c6c294e8e9cbd790bf3c62f03 |
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| 出典メモ | uspto-grants-1985_10 |
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