関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,5 Dibromotoluene | HCID 12006 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 触媒 | Tungsten | HCID 23964 | — |
| 生成物 | 1,4-Dibromo-2-(bromomethyl)benzene | HCID 5326038 | — |
反応手順
33 g (0.1 mole) 2,5-dibromo toluene is placed in a 100 ml three-necked flask, fitted with a reflux condenser, a sealed mechanical stirrer, and a separatory funnel with the stem reaching nearly to the bottom of the flask. The flask is illuminated with two 300-watt tungsten lamps during the reaction. The flask is heated in an oil bath to 150° C., and 18.4 g (5.9 ml, 0.115 mole) bromine is added over two hours. The mixture is stirred for an additional 10 minutes, and the contents, while still liquid, are poured into a 500 ml round-bottom flask containing 300 ml of hot light petroleum ether and 2 g decolorizing carbon. A reflux condenser is attached, and the mixture is heated to reflux until the material dissolves, then rapidly filtered through a pre-heated Buchner funnel. The filtrate is cooled and washed with cold light petroleum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05565543 |
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| 出典データセット | uspto-grants-1996_10 |
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| ORD ID | ord-06440eaa704a44ab983435d709b78aca |
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| 出典メモ | uspto-grants-1996_10 |
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