関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Methyl 5-bromo-2-methylbenzoate | HCID 316201 | — |
| 触媒 | Azobisisobutyronitrile | HCID 6547 | — |
| 溶媒 | (Trifluoromethyl)benzene | HCID 7368 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 5-bromo-2-(bromomethyl)benzoate | HCID 12929136 | 69% |
反応手順
To a solution of methyl 5-bromo-2-methylbenzoate (5.27 g) in trifluoromethylbenzene (50.0 mL) were added AIBN (0.04 g) and N-bromosuccinimide (4.50 g), and the mixture was stirred at 90° C. for 4 hr under argon atmosphere. The reaction mixture was diluted with ethyl acetate, and the mixture was washed with saturated brine. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (4.89 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09315458B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-a7919ee28acd4adba6209dc2b2df2be1 |
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| 出典メモ | uspto-grants-2016_04 |
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