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Hydrochloric Acid → 4-Methyl-2,2-dichloro-1,3-benzodioxole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chlorine | HCID 24526 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 4-Methyl-1,3-benzodioxole | HCID 88560 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 4-Methyl-2,2-dichloro-1,3-benzodioxole | HCID 14405154 | — |
反応手順
160 g of 4-methyl-1,3-benzodioxole are added dropwise to 276 g of phosphorus pentachloride in 840 ml of carbon tetrachloride (prepared from phosphorus trichloride and chlorine), with stirring. Vigorous evolution of hydrogen chloride starts immediately. Towards the end of the reaction, 85 g of chlorine are passed in at about 20° C. and when the evolution of gas has ended, the mixture is then heated under reflux. By distillation, the phosphorus trichloride and carbon tetrachloride are recovered and the 4-methyl-2,2-dichloro-1,3-benzodioxole is then obtained at boiling point: 98-99° C. (22 mbar).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04886816 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-0ce8641352074532a813a695ba1e500a |
| 出典メモ | uspto-grants-1989_12 |