関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenyl-1-naphthylamine | HCID 7013 | — |
| 反応物 | 4,4'-Dibromobiphenyl | HCID 7110 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(4'-bromo-[1,1'-biphenyl]-4-yl)-N-phenylnaphthalen-1-amine | HCID 16755312 | 70% |
反応手順
A mixture of 4,4′-dibromobiphenyl (8.46 g=27.4 mmol), Pd(OAc)2 (105 mg=0.18 mmol), dppf (253 mg=0.46 mmol), N-(1-naphthyl)aniline (2.0 g=9.13 mmol) and sodium t-butoxide (1.32 g=13.7 mmol) in dry toluene was placed in a three-necked flask under a nitrogen atmosphere and stirred at 90° C. for 15 h. After cooling, the reaction was quenched by adding water and then extracted by ethyl acetate. The organic layer was dried over anhydrous MgSO4 and evaporated under vacuum. The products were purified by a silica gel column eluted with hexane. White solid of compound 2N was obtained in 70% yield (2.86 g=6.37 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08183393B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-445ad050c76a4e5ca7eae9f41f26deb5 |
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| 出典メモ | uspto-grants-2012_05 |
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