참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Diazonio-1-ethoxyprop-1-en-1-olate | HCID 53440922 | — |
| 반응물 | HCID 178438709 | HCID 178438709 | — |
| 촉매 | Acetic acid, rhodium(2+) salt | HCID 21674 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | HCID 178438728 | HCID 178438728 | 88.4% |
반응 단계
A mixture of 3′-fluoro-4′-{[4-(trans-4-hydroxycyclohexyl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (3.0 g), rhodium(II) acetate (dimer) (0.027 g) and toluene (30 mL) was heated to 80° C. under an argon atmosphere, a solution of ethyl 2-diazopropionate (3.2 g) in toluene (30 mL) was added dropwise, and the mixture was stirred at 80° C. for 10 min. A solution of ethyl 2-diazopropionate (1.6 g) in toluene (10 mL) was added, and the mixture was stirred at 80° C. for 10 min. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography to give the title compound as a colorless solid (3.2 g, 88%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08921379B2 |
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| 출처 데이터셋 | uspto-grants-2014_12 |
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| ORD ID | ord-cfefed01ceba4973baf51a786e931e2b |
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| 출처 메모 | uspto-grants-2014_12 |
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