関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Dimethoxybenzonitrile | HCID 74842 | — |
| 反応物 | Thioacetamide | HCID 2723949 | — |
| 溶媒 | N,N-dimethylformamide;hydrochloride | HCID 10920465 | — |
| 生成物 | 3,4-Dimethoxythiobenzamide | HCID 2758490 | 61.9% |
反応手順
25 g of 3,4-dimethoxybenzonitrile and 23 g of thioacetamide were dissolved in 120 ml of 10% hydrochloric acid-DMF. The solution was heated at 90° C. for 3 hours. The solution was further heated at 130° C. for 5 hours to conduct a reaction. The solvent was removed by distillation. The residue was washed twice with 100 ml of diethyl ether. Similar washing was conducted with 100 ml of water. The resulting crystals were collected by filtration and dried. Recrystallization from methanol was conducted to obtain 18.7 g of 3,4-dimethoxythiobenzamide as light brown columnar crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06080764 |
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| 出典データセット | uspto-grants-2000_06 |
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| ORD ID | ord-faf2b22a52924dcca2aa946d5eed631b |
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| 出典メモ | uspto-grants-2000_06 |
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