참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phosgene | HCID 6371 | — |
| 반응물 | Phosphonic dichloride, ethenyl- | HCID 74035 | — |
| 반응물 | Poly(vinylphosphonic acid) | HCID 168725 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | (2-Chloroethyl)phosphonic dichloride | HCID 69645 | — |
| 생성물 | Phosphonic dichloride, ethenyl- | HCID 74035 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04548762 |
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| 출처 데이터셋 | uspto-grants-1985_10 |
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| ORD ID | ord-25d1c16c6c294e8e9cbd790bf3c62f03 |
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| 출처 메모 | uspto-grants-1985_10 |
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