関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Fluorene | HCID 6853 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 溶媒 | Propylene Carbonate | HCID 7924 | — |
| 生成物 | 1-Bromo-9h-fluorene | HCID 18694830 | 68% |
反応手順
1.2 litters of propylene carbonate and 160 g (0.96 mol) of fluorene were put into a 2 litter 3-neck round-bottom flask equipped with a stirrer, a thermometer and a reflux condenser under an argon atmosphere, and the resulting mixture was heated to 80° C. so as to make completely dissolved. 179.9 g (1.01 mol) of N-bromosuccinimide was added portionwise to the reaction mixture, and the resultant was stirred at 80° C. for 10 hours. The reaction mixture was cooled down to room temperature to precipitate white solid. The solid was filtered, thoroughly washed with methanol, dried and then recrystallized from ethanol, to obtain white crystal, which was filtered and then sufficiently dried in a vacuum oven at 40° C. to give 160 g (yield: 60%) of the desired product, and its melting point was 102° C.–103° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084231B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-a37453ac498b403e8ea58f83bd8e7af0 |
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| 出典メモ | uspto-grants-2006_08 |
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