関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Thiophenol | HCID 7969 | — |
| 反応物 | Ethyl 2-chloro-4-methyl-1,3-thiazole-5-carboxylate | HCID 594903 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 20364661 | HCID 20364661 | — |
反応手順
Thiophenol (1.90 ml) was dissolved in N,N-dimethylformamide (10 ml) Sodium hydride (60% oil suspension, 740 mg) was added by portions under ice-cooling, and the mixture was stirred at room temperature for 15 min. Thereafter, a solution of ethyl 2-chloro-4-methylthiazole-5-carboxylate (3.05 g) in N,N-dimethylformamide (10 ml) was added dropwise, and the mixture was stirred at the same temperature for 20 min. Water (50 ml) was added to the reaction mixture, and the mixture was extracted with ethyl acetate (50 ml). The ethyl acetate layer was washed twice with water (50 ml) and then with saturated brine (30 ml), and dried (Na2SO4). Ethyl acetate was evaporated under reduced pressure and the obtained residue was purified by column chromatography to give ethyl 4-methyl-2-phenylsulfanylthiazole-5-carboxylate (3.85 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07557123B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-d4501c3e611d4c658621a081bd183b26 |
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| 出典メモ | uspto-grants-2009_07 |
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