関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Octane | HCID 356 | — |
| 反応物 | 2,6-Dichlorobenzoyl chloride | HCID 78392 | — |
| 反応物 | 3,4,5-Trimethoxytoluene | HCID 80922 | — |
| 触媒 | Iron chloride (FeCl3) | HCID 24380 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,6-Dichloro-2',3',4'-trimethoxy-6'-methyl-benzophenone | HCID 22719953 | — |
反応手順
A mixture of 3,4,5-trimethoxytoluene (9.11 g; 50 mmol), octane (25 ml) and iron(III)chloride (50 mg) is stirred at 105° C., and percolating nitrogene 2,6-dichlorobenzoylchloride (12.04 g; 57.5 mmol) is added dropwise within 15 minutes. The mixture is kept at 105° C. and stirred for another 15 minutes. After cooling to 50° C. ethylacetate (50 ml) is added, the mixture shaken twice with 2N hydrochloric acid, once with water and dried. The ethylacetate is evaporated (70° C.) and the liquid cooled with stirring. At 50° C. petrolether (50 ml) is added. The white crystals formed are sucked off, washed with petrolether and dried. Yield 12.55 g (70.7%), mp. 92° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05866722 |
|---|
| 出典データセット | uspto-grants-1999_02 |
|---|
| ORD ID | ord-6e7b4119066c40779be23be71e686774 |
|---|
| 出典メモ | uspto-grants-1999_02 |
|---|
