참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trimethylsilyl triflate | HCID 65367 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Ethanone, 1-[3-methyl-4-(phenylmethoxy)phenyl]- | HCID 12969325 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-[4-(Benzyloxy)-3-methylphenyl]-2-bromoethanone | HCID 12969327 | 70.2% |
반응 단계
To a solution of 1-(4-benzyloxy-3-methyl-phenyl)-ethanone (12.89 g; 53.1 mmol) in CH2Cl2 was added, dropwise, at 0° C., DIPEA (10.9 mL; 63.7 mmol) and trimethylsilyl trifluoromethanesulfonate (11.1 mL; 61.1 mmol). The resulting mixture was stirred at 0° C. for 1 hour, and subsequently, NBS (10.87 g; 61.1 mmol) was added in one portion. The mixture was allowed to warm to RT stirred overnight. Then the mixture was concentrated in vacuo, the residue dissolved in EtOAc, washed with water twice, and brine, dried (MgSO4), filtered, and concentrated in vacuo to afford 1-(4-benzyloxy-3-methyl-phenyl)-2-bromo-ethanone (11.90 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09273017B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_03 |
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| ORD ID | ord-fe1b9589b55747c4ba87726a178f5938 |
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| 출처 메모 | uspto-grants-2016_03 |
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