참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Azobisisobutyronitrile | HCID 6547 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | 4-Methylperfluorobiphenyl | HCID 58782894 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 생성물 | 4-Bromomethylperfluorobiphenyl | HCID 86591121 | 60% |
반응 단계
A mixed solution of a mixture comprising the 4-methylperfluorobiphenyl mentioned above, an N-bromo succinic imide (NBS) (26.7 g, 150 mmol), AIBN (0.99 g, 6 mmol) and a carbon tetrachloride (100 mL) was subjected to heating under reflux for 1 week. During this process, the progress of the reaction was confirmed by TLC, and NBS and AIBN were added on a timely basis. Ultimately, 285 mmol NBS and 15 mmol AIBN were added to the solution. After the reaction was completed, the solution was cooled to room temperature, and the solvent was removed under reduced pressure. The crude product was purified by silica gel column chromatography (developing solvent: hexane-ethyl acetate=100:1), and the 4-(bromomethyl)perfluorobiphenyl (7.36 g, 18 mmol, total yield from methyl lithium 60%) was isolated.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07193113B2 |
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| 출처 데이터셋 | uspto-grants-2007_03 |
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| ORD ID | ord-4b0ac3c02c7743b1a278c08395d09e75 |
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| 출처 메모 | uspto-grants-2007_03 |
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