関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | 2,5-Dimethylaniline | HCID 7259 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 触媒 | Cupric Chloride | HCID 24014 | — |
| 生成物 | 4-Amino-2,5-dimethylbenzaldehyde | HCID 55284692 | 22.8% |
反応手順
6.06 g (50.0 mmol) of 2,5-dimethylaniline are initially charged in 1000 ml of DMSO, 13.55 g (100.0 mmol) of copper(II) chloride are added and concentrated hydrochloric acid is then added slowly. The reaction mixture is heated at 90° C. for 3 h and then added to ice-water. After addition of aqueous sodium hydroxide solution, the mixture is filtered and extracted repeatedly with ethyl acetate, and the combined organic phases are dried over Na2SO4 and freed from solvent under reduced pressure. The crude product is purified by column chromatography. (2.27 g, purity 75.0%, yield 22.8%, log P (pH 2.3)=1.34).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08334237B2 |
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| 出典データセット | uspto-grants-2012_12 |
|---|
| ORD ID | ord-ba5b549cf843458db48e0963abeacaa2 |
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| 出典メモ | uspto-grants-2012_12 |
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