関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Iodobiphenyl | HCID 15322 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl | HCID 11269872 | — |
| 反応物 | 2,4-Diphenylaniline | HCID 12316638 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 生成物 | N-([1,1'-biphenyl]-4-yl)-[1,1':3',1''-terphenyl]-4'-amine | HCID 86762383 | 840.5% |
反応手順
Xylene (250 mL) was bubbled with nitrogen for 15 min, followed by addition of 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (1.8 g, 4.4 mmol) and Pd2(dba)3 (1.0 g, 1.1 mmol). The mixture was bubbled with nitrogen for 15 min, then [1,1′:3′,1″-terphenyl]-4′-amine (9.8 g, 40.0 mmol), 4-iodobiphenyl (10.3 g, 36.7 mmol), sodium tert-butoxide (7.0 g, 73.4 mmol) were added. The mixture was bubbled with nitrogen for 15 min and refluxed for 13 h. After cooling, the reaction mixture was filtered through a silica pad and washed with toluene. The solvent was removed in vacuo and the residue was purified by flash chromatography using 40-60% toluene/hexane to afford N-([1,1′-biphenyl]-4-yl)-[1,1′:3′,1″-terphenyl]-4′-amine (14.7 g, 92% yield) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08716484B1 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-7e5407e0152849ab8e1f57f1f6b24da6 |
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| 出典メモ | uspto-grants-2014_05 |
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