関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethylsilyl triflate | HCID 65367 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Ethanone, 1-[3-methyl-4-(phenylmethoxy)phenyl]- | HCID 12969325 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[4-(Benzyloxy)-3-methylphenyl]-2-bromoethanone | HCID 12969327 | 70.2% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09045441B2 |
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| 出典データセット | uspto-grants-2015_06 |
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| ORD ID | ord-9622c99e8fab4e0983639e99693eccf2 |
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| 出典メモ | uspto-grants-2015_06 |
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