Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 556937생성일: 2026년 10월 25일
Ethanol → 4-(4-Chlorophenyl)-1-[3-(5,11-dihydro-7-ethoxycarbonyl-[1]benzoxepino[2,3-b]pyridin-5-ylidene) propyl]piperidine-4-ol
https://huagongshe.com/reaction/556937
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| 반응물 | 4-(4-Chlorophenyl)-1-[3-(5,11-dihydro-7-trifluoromethanesulfonyloxy[1]benzoxepino[2,3-b]pyridin-5-ylidene)propyl]piperidin-4-ol | HCID 73455970 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 생성물 | 4-(4-Chlorophenyl)-1-[3-(5,11-dihydro-7-ethoxycarbonyl-[1]benzoxepino[2,3-b]pyridin-5-ylidene) propyl]piperidine-4-ol | HCID 66758683 | 73% |
반응 단계
The compound of Example 169 (0.166 g) was dissolved in DMF (1 mL) and treated with palladium (II) acetate (0.007 g), 1,3-bis-diphenylphosphinopropane (0.012 g), triethylamine (0.1 mL) and ethanol (1 mL), and stirred at 60° C. for 18 hours under a CO balloon. The resulting solution was quenched with water, extracted with ethyl acetate, concentrated in vacuo, and purified by silica gel chromatography (87:10:3 ethyl acetate:methanol:triethylamine). The residue was further purified by chromatography on a reverse-phase solid-phase-extraction column, eluting with water-acetonitrile, 0.1% formic acid, to yield 0.114 g (73%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08058287B2 |
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| 출처 데이터셋 | uspto-grants-2011_11 |
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| ORD ID | ord-4b8e4a41e57c4c22b37ef4cba85338e2 |
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| 출처 메모 | uspto-grants-2011_11 |
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