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Styrene → (1,1,3-Trichloro-3-phenylpropyl)phosphonic dichloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Styrene | HCID 7501 | — |
| 反応物 | (Trichloromethyl)phosphonic dichloride | HCID 277422 | — |
| 反応物 | Triethylazanium chloride | HCID 12698378 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (1,1,3-Trichloro-3-phenylpropyl)phosphonic dichloride | HCID 21399673 | — |
反応手順
11.8 g (0.05 mole) trichloromethane phosphonic dichloride, 7.8 g (0.075 mole) styrene, 134 mg (1 mmole) anhydrous cupric chloride and 206 mg triethylammonium chloride were brought into solution by 5 ml acetonitrile, and heated in the absence of air in a sealed ampoule at 110° during 3.5 hours. After cooling and opening of the ampoule, the reaction mixture was subjected to fractionation in vacuo, through a short Vigreux column. 9.1 g pure 1:1 adduct, 1,1,3-trichloro-3-phenyl-propane-1-phosphonic dichloride was obtained bp/0.05: 121°. Found: Cl: 50.8, Calc. for C9H8Cl5OP: 52.1%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04057578 |
| 出典データセット | uspto-grants-1977_11 |
| ORD ID | ord-e8bc554633f140549bd5366045338224 |
| 出典メモ | uspto-grants-1977_11 |