참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Chlorodiphenylphosphine | HCID 66180 | — |
| 반응물 | (2-Bromo-1-phenylcyclopropyl)benzene | HCID 282328 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,2-Diphenyl-1-(diphenylphosphino)-1-methylcyclopropane | HCID 21909130 | 50% |
반응 단계
Under a nitrogen atmosphere, 1-bromo-2,2-diphenylcyclopropane (1.44 g, 5.0 mmol) and magnesium (0.134 g, 5.5 mmol) and THF (10 ml) were placed in a reaction flask. Then, a trace amount of iodine was added and the mixture was stirred at 40° C. for 2 hours. After cooling, copper iodide (0.961 g, 5.0 mmol) and chlorodiphenylphosphine (0.90 ml, 5.0 mmol) were added and the resulting mixture was stirred at 40° C. for 20 hours. After cooling to room temperature, hexane (10 ml) was added to the reaction mixture, and crystal separated was then collected by filtration. The crystal was dissolved in toluene, washed with an aqueous 28% ammonia solution and a brine, and dried over anhydrous magnesium sulfate. The solvent was then removed under reduced pressure and the concentrate was recrystallized from a mixture of methanol and toluene to give the title compound (0.98 g, 50%) as white crystal.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07129367B2 |
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| 출처 데이터셋 | uspto-grants-2006_10 |
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| ORD ID | ord-3d2a9b07df3147e3a5fcf8e9e22630ad |
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| 출처 메모 | uspto-grants-2006_10 |
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