関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-Iodophenol | HCID 10894 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(3-Chloro-propionylamino)-thiophene-3-carboxylic acid methyl ester | HCID 68686721 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[2-(4-Iodo-phenoxy)-acetylamino]-thiophene-3-carboxylic acid methyl ester | HCID 68687330 | 99.5% |
反応手順
To a solution of 4-(3-chloro-propionylamino)-thiophene-3-carboxylic acid methyl ester ([51486-30-7], 2.0 g, 8.6 mmol) in dimethylformamide (30 mL) was added potassium carbonate (1.77 g, 12.8 mmol) and 4-iodophenol (2.26 g, 10.3 mmol) and the reaction mixture was then stirred overnight at 90° C. To the reaction mixture was added ethyl acetate (approximately 30 mL). The solid was filtered and washed with ethyl acetate. The filtrate was then reduced in vacuo and dissolved in dichloromethane (approximately 50 mL). The solution was filtered again over charcoal and to the filtrate was added isopropylether. After reducing the solution slowly in vacuo the solid was filtered to yield the title compound (3.57 g, 79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732452B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-359696935bbe465abbd89b8f25825cb3 |
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| 出典メモ | uspto-grants-2010_06 |
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