関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Fluoreneone | HCID 22281833 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 触媒 | Sulfuric Acid | HCID 1118 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Bromofluorenone | HCID 66810654 | 92.9% |
反応手順
In a three-liter flask having four openings equipped with a stirrer, a thermometer, a dropping funnel, and a reflux condenser, respectively, 256 g (1.4 mol) of fluorenone, 1 L of water, three drops of a surfactant, and five drops of sulfuric acid were placed and stirred to mix. By adding 250 g (1.6 mol) of bromine into the mixture, a reaction was started. After the reaction had been conducted at 50° C. for 12 hours, unreacted bromine was decomposed with an aqueous solution of sodium hydrogen sulfite. The reaction product, which was a dark yellow solid, was filtered and thus 365 g of a crude product was obtained. The crude product was dissolved in toluene and was subsequently washed with water and a sodium hydrogencarbonate aqueous solution. The resulting organic liquid was dried using anhydrous magnesium sulfate. After filtration, the liquid was concentrated and then allowed to stand at 0° C., so that a yellow solid was precipitated. The precipitate was filtered and subsequently washed with toluene, followed by drying. Thus, 339 g (1.3 mol, yield of 92%) of a yellow solid product was obtained. This product was subjected to gas chromatography and the purity of the product was 99.4%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06858764B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-4896137c19754718b0fb141a71c5dfc7 |
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| 出典メモ | uspto-grants-2005_02 |
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