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Chlorobenzene → 4-Chlorophenyldichlorophosphine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorobenzene | HCID 7964 | — |
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | 4-Chlorophenyldichlorophosphine | HCID 295605 | — |
反応手順
To a suspension of 53.3 g (0.4 mol) of aluminium chloride in 40 ml (0.39 mol) of chlorobenzene, 104.8 ml (1.2 mol) of phosphorus trichloride are added dropwise at ambient temperature. The reaction mixture is refluxed for three hours. Then within 30 minutes 37.2 ml (0.4 mol) of phosphorus oxychloride are added dropwise at 83° C. After 12 hours at ambient temperature the residue is stirred with petroleum ether and decanted off. The combined organic extracts are distilled under high vacuum at 57-61° C. and 0.048-0.035 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06114532 |
| 出典データセット | uspto-grants-2000_09 |
| ORD ID | ord-7225f06a17024e97a5aa8415d64641c1 |
| 出典メモ | uspto-grants-2000_09 |