関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloride | HCID 312 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 4-Chlorotetrahydrophthaloyl chloride | HCID 19746828 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 4-Chlorobenzene-1,2-dicarbonyl dichloride | HCID 15044562 | — |
反応手順
To a 1-l three-necked flask, equipped with a mechanical stirrer, a condenser with a gas outlet and an equa-pressured addition funnel, is charged 241.5 g (1 mole) of 4-chloratetrahydrophthaloyl chloride and 36 g of chlorobenzene. The mixture is heated to 100°-110° C. with stirring. Bromine, 320 g (2 moles) is added dropwise into the solution in a sub-surface manner. The color dissipates quickly and an evolution of gas occurs. When approximately 240 g of bromine has been added, the pot temperature is raised to 135° C. The addition of bromine continues until completion. The pot temperature is then raised to 165°-170° C. for 2-4 fours. during this period, an additional amount of bromine, such as about 10 to 15 g, may be added to complete the conversion of 4-chlorotetrahydrophthaloyl chloride. A good yield of 4-chlorophthaloyl chloride will be obtained from the distillation of the mixture.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05049682 |
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| 出典データセット | uspto-grants-1991_09 |
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| ORD ID | ord-57649898f521463fbe85bc2449cf9fab |
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| 出典メモ | uspto-grants-1991_09 |
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