참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | 1-Bromooctane | HCID 8140 | — |
| 반응물 | 2-Bromo-9H-fluorene | HCID 14336 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 촉매 | Benzyl triethylammonium chloride | HCID 66133 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Diethylether water | HCID 21584184 | — |
| 생성물 | 2-Bromo-9,9-di-n-octylfluorene | HCID 12964693 | 155.4% |
반응 단계
A 3 L flask fitted with a mechanical stirrer was charged with 2-bromofluorene (45 g, 183.6 mmole) and 150 mL DMSO. Under a N2 atmosphere was added 80 mL of a 50% aqueous NaOH solution and 2.72 g of benzyltriethylammonium chloride (2.72 g, 11.98 mmole). This was stirred for 2 h at RT. With vigorous mechanical stirring, n-octylbromide (84.96 g, 440 mmole) was added via a dropping funnel (exotherm). Stirring was continued for 2 hours. To the reaction mixture was added 500 mL of a 1:1 mixture of water/ether, and the organic layer separated and was washed successively with brine and then water. Drying over magnesium sulfate and evaporation of the solvent gave an oil. Purification by column chromatography (silica gel; hexane as the mobile phase) gave 67 g (78% yield) of 2-bromo-9,9-dioctylfluorene as a pale oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07271406B2 |
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| 출처 데이터셋 | uspto-grants-2007_09 |
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| ORD ID | ord-2c83e6d3ede0462f8faadbb22600d502 |
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| 출처 메모 | uspto-grants-2007_09 |
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