참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Fluorene | HCID 6853 | — |
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | Sodium Bisulfite | HCID 23665763 | — |
| 촉매 | Sulfuric Acid | HCID 1118 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 2-Bromo-9H-fluorene | HCID 14336 | 82% |
반응 단계
In a three-liter flask having four openings equipped with a stirrer, a thermometer, a dropping funnel, and a reflux condenser, respectively, 237 g (1.4 mol) of fluorene, 1 L of water, three drops of a surfactant, and five drops of sulfuric acid were placed and stirred to mix. By adding 230 g (1.4 mol) of bromine into the mixture, a reaction was started. After the reaction had been conducted at room temperature for 5 hours, unreacted bromine was decomposed with an aqueous solution of sodium hydrogen sulfite. The reaction product, which was a light yellow solid, was filtered and thus 334 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 white solid was precipitated. The precipitate was filtered and subsequently washed with toluene, followed by drying. Thus, 287 g (1.1 mol, yield of 82%) of a white solid product was obtained. This product was subjected to gas chromatography and the purity of the product was 98.8%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06858764B2 |
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| 출처 데이터셋 | uspto-grants-2005_02 |
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| ORD ID | ord-0756538c8d9f4afa86698da3925b6c16 |
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| 출처 메모 | uspto-grants-2005_02 |
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