참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | (Z)-1-Ethoxy-2-(tributylstannyl)ethene | HCID 2763294 | — |
| 반응물 | 3,9-Dibromo-5,7-dihydrodibenzo[c,e]oxepine | HCID 22316165 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2-Bromo-1-(9-bromo-5,7-dihydro-dibenzo[c,e]oxepin-3-yl)-ethanone | HCID 59610296 | 25.2% |
반응 단계
To the solution of 3,9-dibromo-5,7-dihydro-dibenzo[c,e]oxepine (416 mg, 1.2 mmol) and tributyl(ethoxyvinyl)stannane (878 μl, 2.6 mmol) in dioxane (6 ml) was added PdCl2(PPh3)2 (30 mg). The mixture was heated at 80° C. for 16 hours and was cooled to 0° C. Water (2 ml) was added, followed by slow addition of NBS (464 mg, 2.6 mmol) over 5 minutes period. The mixture was stirred at 0° C. for additional 40 minutes, and the solvent was removed under reduced pressure. The mixture was diluted with EtOAc, and was washed with water and brine and dried with sodium sulfate. Concentration and purification by flash column chromatography (hexane/EtOAc) gave 2-bromo-1-(9-bromo-5,7-dihydro-dibenzo[c,e]oxepin-3-yl)-ethanone (120 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08822430B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-204059ad810a405b91c94d219535ca97 |
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| 출처 메모 | uspto-grants-2014_09 |
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