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Water → 2,3-Dichloro-4,5-dimethoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methane, dichloromethoxy- | HCID 21004 | — |
| 反応物 | 1,2-Dichloro-3,4-dimethoxybenzene | HCID 56061 | — |
| 触媒 | Titanium tetrabromide | HCID 123263 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,3-Dichloro-4,5-dimethoxybenzaldehyde | HCID 14748634 | 76.2% |
反応手順
105.2 g of dichloromethoxymethane are added to a solution of 122.6 g of 1,2-dichloro-3,4-dimethoxybenzene in methylene chloride, and titanium tetrabromide is added dropwise to the mixture at -50° to -60° C. The mixture is stirred at room temperature for 20 hours. The reaction mixture is poured into water and the organic layer is separated. The aqueous layer is extracted with chloroform, and the extract and the above-obtained organic layer are combined. The mixture is washed with water, dried and evaporated to remove solvent. The residue is washed with n-hexane to give 106 g of 2,3-dichloro-4,5-dimethoxybenzaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04965282 |
| 出典データセット | uspto-grants-1990_10 |
| ORD ID | ord-ade9d4bb5d6b4a02a98c6250dc8a38bc |
| 出典メモ | uspto-grants-1990_10 |