関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | (2-Bromo-1-phenylcyclopropyl)benzene | HCID 282328 | — |
| 反応物 | Chlorodiisopropylphosphine | HCID 538967 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,2-Diphenyl-1-(diisopropylphosphino)-1-methylcyclopropane | HCID 21909135 | 66% |
反応手順
Under a nitrogen atmosphere, 1-bromo-2,2-diphenylcyclopropane (1.43 g, 5.0 mmol), magnesium (0.133 g, 5.5 mmol) and THF (10 ml) were placed in a reaction flask, followed by addition of a trace amount of iodine and stirring at 40° C. for 1.5 hours. After cooling, copper iodide (0.952 g, 5.0 mmol) and chlorodiisopropylphosphine (0.80 ml, 5.0 mmol) were added and the resulting mixture was stirred at 40° C. for 5 hours, followed by cooling to room temperature. The resulting mixture was diluted with hexane (20 ml) and crystal separated was collected by filtration. The crystal was dissolved in toluene, and the toluene solution was washed with a 28% aqueous ammonia and a brine, and dried over anhydrous magnesium sulfate. Then, the solvent was removed under reduced pressure to give the title compound (1.06 g, 66%) as white crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07129367B2 |
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| 出典データセット | uspto-grants-2006_10 |
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| ORD ID | ord-c365289a83e448169295659bb3949063 |
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| 出典メモ | uspto-grants-2006_10 |
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