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2-Methyl-8-hydroxyquinoline → 8-Hydroxy-2-quinolinecarboxaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methyl-8-hydroxyquinoline | HCID 13224 | — |
| 反応物 | Selenium Dioxide | HCID 24007 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 8-Hydroxy-2-quinolinecarboxaldehyde | HCID 599342 | — |
反応手順
8-hydroxy-2-methylquinoline (2 g, 12.4 mmol.), selenium dioxide (1.74 g, 15.8 mmol), 300 ml of pre-dried 1,4-dioxane, and 1.5 ml of water were mixed and stirred in a 1-L round bottom flask. The resulting solution was then refluxed for 24 h. The reaction was monitored until completion using TLC method. The reaction mixture was then filtered off, and the selenium metal was then washed with dichloromethane, and the combined filtrates were then evaporated off under reduced pressure. The crude product was then purified by sublimation under reduced pressure or by silica gel column chromatography to yield pure yellow needle crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09321730B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-461ea512d4c045988b4084611ea958cb |
| 出典メモ | uspto-grants-2016_04 |