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Potassium Carbonate → 2-Mercapto-6-(3,4-dimethoxyphenyl)-4-methyl-pyridine-3-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(3,4-Dimethoxyphenyl)butane-1,3-dione | HCID 368060 | — |
| 反応物 | 2-Cyanoethanethioamide | HCID 1416277 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2-Mercapto-6-(3,4-dimethoxyphenyl)-4-methyl-pyridine-3-carbonitrile | HCID 178488562 | 98.4% |
反応手順
5.0 g (22.5 mmol) 1-(3,4-dimethoxyphenyl)butane-1,3-dione, 2.9 g (29.2 mmol) cyanthioacetamide and 4.0 g (29.2 mmol) potassium carbonate are added by stirring to 170 ml acetone at room temperature for 21 h. Then, the solvent is removed and the residue is just dissolved in ethanol/water (1:1). Following acidification with glacial acetic acid, the resulting precipitate is sucked off, washed with some water, suck dried and dried in vacuo at 50° C. 6.34 g (98%) 2-mercapto-6-(3,4-dimethoxyphenyl)-4-methyl-pyridine-3-carbonitrile is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08058285B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-c19656c7d9f34cc5a27608dd7eb91648 |
| 出典メモ | uspto-grants-2011_11 |