関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 5-Bromo-1,3-difluoro-2-iodobenzene | HCID 2782702 | — |
| 反応物 | HCID 178444242 | HCID 178444242 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 178444293 | HCID 178444293 | 39.1% |
反応手順
First, 50 ml of ethanol containing 5.61 g of 4-(trans-4-pentylcyclohexyl)phenylboronic acid dissolved therein, 50 ml of benzene containing 5.0 g of 4-bromo-2,6-difluoro-1-iodobenzene dissolved therein, 15.7 ml of a sodium carbonate aqueous solution with a concentration of 2.0 mol/l, and 0.45 g of tetrakis(triphenylphosphine)palladium(0) were put in an argon-replaced 200 ml flask, and stirred under reflux for 48 hours. After the reaction, water and ether were added to the reaction solution for extraction. The resultant ether layer was washed with a saturated brine and dried with sodium sulfate. The solvent was then distilled off. The residue was purified by silica gel column chromatography (eluent:hexane) and recrystallized from acetone, to obtain 2.58 g (Y: 39.1%) of 4-bromo-2,6-difluoro-4′-(trans-4-pentylcyclohexyl)biphenyl. The purity of the resultant compound was 100.0% as measured by GC. (5-b) Synthesis of polymerizable compound 2,6-difluoro-4′-(trans-4-pentylcyclohexyl)-4-vinylbiphenyl represented by formula (E) above
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06388146B1 |
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| 出典データセット | uspto-grants-2002_05 |
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| ORD ID | ord-66da78fe7e7f4b39a300355dfbd4cd1d |
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| 出典メモ | uspto-grants-2002_05 |
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