関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Aminocyclohexanecarboxylic acid | HCID 1366 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Furancarbonyl chloride | HCID 68242 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[(2-Furanylcarbonyl)amino]cyclohexanecarboxylic acid | HCID 17455254 | 237.3% |
反応手順
71.6 g (0.5 mol) of 1-aminocyclohexanecarboxylic acid was added to a solution of 20 g (0.5 mol) of sodium hydroxide in 250 ml of water, and the mixture was stirred at 80° C. for 2 hours. The mixture solution was cooled by ice-water, 71.8 g (0.2 mol) of 2-furancarbonyl chloride and a solution of 24 g (0.6 mol) of sodium hydroxide in 100 ml of water were simultaneously added thereto over approximately 1 hour. The reaction solution was slowly returned to room temperature and stirred overnight. After 80 ml of ethyl acetate was added to the reaction solution and the mixture was stirred for 1 hour, the insolubles were removed by filtration. The aqueous layer was separately collected, 49 ml of concentrated hydrochloric acid was added thereto under ice-cooling. The precipitated crystal was collected by filtration and dried-under reduced pressure to obtain 112.6 g (95%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829209B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-d2bb77af91dd4b7eae884941754e58c0 |
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| 出典メモ | uspto-grants-2014_09 |
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