참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-Ethoxy-4-ethynylbenzene | HCID 2775124 | — |
| 반응물 | N-[2-(5-bromo-pyridin-2-yl)-ethyl]-acetamide | HCID 66611273 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | N-{2-[5-(4-Ethoxy-phenylethynyl)-pyridin-2-yl]-ethyl}-acetamide | HCID 68181171 | — |
반응 단계
0.55 mL (3.91 mmol) DIPEA is added to 190 mg (0.78 mmol) N-[2-(5-bromo-pyridin-2-yl)-ethyl]-acetamide (I48.1), 3.72 mg (0.02 mmol) CuI and 13.7 mg (0.02 mmol) bis(triphenylphosphin)palladium-(II)-chloride. 171 mg (1.17 mmol) 4-ethoxyphenylacetylene are added and the reaction mixture is heated for 10 min at 80° C. in a microwave oven. The mixture is diluted with EtOAc and washed with water (1×) and diluted aq. ammonia solution. The organic layer is dried with MgSO4 and the solvent is removed in vacuo. The residue is purified by HPLC (MeOH/H2O/NH3).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08835472B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-51640ff832fb4083add4a8d495683a8a |
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| 출처 메모 | uspto-grants-2014_09 |
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