関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-methyl-N-(4-methylphenyl)-1,2,3-thiadiazole-5-carboxamide | HCID 850826 | — |
| 反応物 | 4-Morpholinesulfenyl chloride | HCID 12297779 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-methyl-N-(4-methylphenyl)-N-morpholinothio-1,2,3-thiadiazole-5-carboxamide | HCID 15906625 | 52% |
反応手順
To 10 ml of methylene chloride were added 0.50 g (2.1 mmol) of 4-methyl-N-(4-methylphenyl)-1,2,3-thiadiazole-5-carboxamide and 0.50 g (3.3 mmol) of N-(chlorosulfenyl)morpholine. Then, 0.33 g (3.3 mmol) of triethylamine was slowly added thereto, and the resulting mixture was reacted with stirring for 5 hours. After the reaction was completed, the reaction mixture containing the objective product was poured into water, the objective product was extracted with ethyl acetate, the organic layer was washed with water and dried on anhydrous sodium sulfate, the solvent was distilled off under reduced pressure, and the crude crystal thus obtained was washed with ether. As a result, 0.38 g of the objective compound was obtained (Property: m.p. 60° C. (decomposed); Yield: 52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06348460B1 |
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| 出典データセット | uspto-grants-2002_02 |
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| ORD ID | ord-9cc0f3aa999e4288ac25e7d0812b3bd0 |
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| 出典メモ | uspto-grants-2002_02 |
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