참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Iodonaphthalene | HCID 7004 | — |
| 반응물 | 4-Pentyn-1-ol | HCID 79346 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Diethylamine | HCID 8021 | — |
| 생성물 | 5-(1-Naphthyl)-4-pentyn-1-ol | HCID 19955557 | 68.7% |
반응 단계
Under a nitrogen atmosphere, a mixture of 4.0 mL (0.027 mole) of 1-iodonaphthalene, 0.1 gram (0.0003 mole) of copper(I) iodide, and 0.19 gram (0.0003 mole) of bis(triphenylphosphine)palladium(II) chloride in 75 mL of diethylamine was stirred, and 2.6 mL (0.027 mole) of 4-pentyn-1-ol was added in one portion. Upon completion of addition, the reaction mixture was stirred at ambient temperature for about 18 hours. Gas chromatographic (GC) analysis of the reaction mixture indicated that the reaction had not gone to completion. An additional 0.5 mL of the 4-pentyn-1-ol was added, and the reaction mixture was stirred for an additional six hours. GC analysis of the reaction mixture indicated that the reaction was complete. The reaction mixture was passed through a column of silica gel. Elution was accomplished using methylene chloride. The eluate was concentrated under reduced pressure, yielding 3.9 grams of 5-(naphth-1-yl)-4-pentyn-1-ol. The NMR spectrum was consistent with the proposed structure.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05521192 |
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| 출처 데이터셋 | uspto-grants-1996_05 |
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| ORD ID | ord-0e2091d86477426185264f1752389d97 |
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| 출처 메모 | uspto-grants-1996_05 |
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