関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Aminobiphenyl | HCID 7015 | — |
| 反応物 | 4-Iododibenzofuran | HCID 458257 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl | HCID 11269872 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 生成物 | N-[1,1'-Biphenyl]-2-YL-4-dibenzofuranamine | HCID 68904161 | 837.7% |
反応手順
Toluene (250 mL) was bubbled with nitrogen for 15 min, followed by addition of 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (1.7 g, 4.2 mmol), and Pd2(dba)3 (1.0 g, 1.1 mmol). The mixture was bubbled with nitrogen for 15 min, then [1,1′-biphenyl]-2-amine (3.4 g, 20.0 mmol), 4-iododibenzo[b,d]furan (10.3 g, 35.0 mmol), and sodium tert-butoxide (6.7 g, 70.0 mmol) were added. The mixture was bubbled with nitrogen for 15 min and refluxed for 24 h. After cooling, the reaction mixture was filtered through a silica pad and washed with DCM. The solvent was removed in vacuo and the residue was purified by flash chromatography using 25% DCM/hexane (containing 0.75% triethylamine) to yield N-([1,1′-biphenyl]-2-yl)dibenzo[b,d]furan-4-amine (11.8 g, 98% yield) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09293712B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-a43bcae1d0cb4982a89c74011ebd7937 |
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| 出典メモ | uspto-grants-2016_03 |
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