참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromobenzene | HCID 7961 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 2-Methyl-6-(3-piperidin-4-ylideneprop-1-ynyl)pyridine | HCID 87550402 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 촉매 | Binap, (A+-)- | HCID 634876 | — |
| 생성물 | 2-Methyl-6-[3-(1-phenylpiperidin-4-ylidene)prop-1-ynyl]pyridine | HCID 25183826 | 100% |
반응 단계
A mixture of the compound of Example 3 (0.22 g, 1.04 mmol), bromobenzene (0.17 g, 1.04 mmol), cesium carbonate (0.68 g, 2.1 mmol), BINAP (0.031 g, 0.05 mmol), palladium(II)acetate (0.01 mg, 0.05 mmol), in anhydrous and degassed toluene (10 mL) was heated at 110° C. under a nitrogen atmosphere for 12 h in a sealed vessel. The reaction mixture was cooled, poured into water and extracted with EtOAc. The combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to afford a residue, which was purified by flash chromatography (EtOAc—Petroleum Ether 2:8) affording the title product (0.30 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08518916B2 |
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| 출처 데이터셋 | uspto-grants-2013_08 |
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| ORD ID | ord-25430e53cc9c41d1a5f6276ae8efe333 |
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| 출처 메모 | uspto-grants-2013_08 |
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