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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 3,5-Dichloro-4-hydroxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone | HCID 6775 | — |
| 反応物 | Benzenemethanol, 3,5-dichloro-4-hydroxy- | HCID 176409 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3,5-Dichloro-4-hydroxybenzaldehyde | HCID 16839 | 22% |
反応手順
2,6-Dichloro-4-hydroxymethylphenol (3.56 g, 18.4 mmol) was dissolved in dioxane, and DDQ (4.19 g, 18.4 mmol) was added. The reaction mixture was stirred at rt overnight. The solvents were removed under reduced pressure. The residue was diluted with CH2Cl2, and the mixture was filtered. The filtrate was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Crystallization from EtOAc yielded the title compound (0.77 g, 22%). LC-MS: tR=0.82 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08138340B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-771dbcb00c9447bc92e7895d8fa37ff7 |
| 出典メモ | uspto-grants-2012_03 |