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 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(4'-bromo-[1,1'-biphenyl]-4-yl)-N-phenylnaphthalen-1-amine | HCID 16755312 | 62% |
反応手順
A mixture of N-phenylnaphthalen-1-amine (4.41 g, 20 mmol), 4,4′-dibromo-1,1′-biphenyl (15 g, 48 mmol), sodium tert-butoxide (4.8 g, 50 mmol) and Pd(dppf)Cl2 (0.44 g, 0.6 mmol) in anhydrous toluene (100 ml) was degassed and heated at 80° C. for 10 hours. After cooling to RT, the mixture was poured into dichloromethane (400 ml) and stirred for 30 min, then washed with brine (100 ml). The organic is collected and dried over Na2SO4, loaded on silica gel, and purified by flash column (hexanes to hexanes/ethyl acetate 90:1) to give a solid which was washed with methanol and dried under air to give a white solid 4 (5.58 g, in 62% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09373797B2 |
|---|
| 出典データセット | uspto-grants-2016_06 |
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| ORD ID | ord-324a2aa143414f499e1c6b4e39b8bb50 |
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| 出典メモ | uspto-grants-2016_06 |
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