関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | 7-Methylquinoline | HCID 11927 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7-Quinolinemethanol | HCID 97609 | 3% |
反応手順
To a solution of 7-methylquinoline (2.86 g) in ethyl acetate (100 mL) were added N-bromosuccinimide (3.56 g) and 2,2′-azobis(isobutyronitrile) (197 mg) at room temperature, and the mixture was refluxed for 1.5 hr. The reaction mixture was allowed to cool to room temperature, and washed with water. The obtained organic layer was concentrated under reduced pressure, to the residue were added DME (200 mL), water (100 mL), and silver carbonate (27.6 g), and the mixture was stirred at room temperature for 20 hr. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/methanol), and then purified by NH silica gel column chromatography (ethyl acetate/hexane) to give the title compound (94 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08883788B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-4687f1df1c0448c09811688c8d7dd398 |
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| 出典メモ | uspto-grants-2014_11 |
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