참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Lithium Bromide | HCID 82050 | — |
| 반응물 | Di-tert-butylchlorophosphine | HCID 139566 | — |
| 반응물 | (2-Bromo-1-phenylcyclopropyl)benzene | HCID 282328 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Di-tert-butyl(1-methyl-2,2-diphenylcyclopropyl)phosphane | HCID 21909131 | 47% |
반응 단계
Under a nitrogen atmosphere, 1-bromo-2,2-diphenyl-cyclopropane (1.44 g, 5.0 mmol), magnesium (0.134 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 one hour. After cooling, copper iodide (0.962 g, 5.0 mmol), lithium bromide (0.567 g, 6.5 mmol) and chlorodi-tert-butylphosphine (0.95 ml, 5.0 mmol) were added and the resulting mixture was stirred at 60° C. for 3 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. The solvent was then removed under reduced pressure to give the title compound (0.83 g, 47%) 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-aec168b5a6f641b3bf59928e3e57392e |
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| 출처 메모 | uspto-grants-2006_10 |
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