関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenyl isocyanate | HCID 7672 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-(1-Aminocyclohexyl)acetic acid hydrochloride | HCID 4426693 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | {1-[(Anilinocarbonyl)amino]cyclohexyl}acetic acid | HCID 57847120 | 55.7% |
反応手順
To a solution of (1-aminocyclohexyl)acetic acid (0.232 mg, 1.48 mmol) in a mixture of 1,4-dioxane (9 ml) and water (3 ml) was added 30% aqueous sodium hydroxide solution to pH 9. Phenylisocyanate (0.24 ml, 2.22 mmol) was added dropwise at 35° C. and 30% aqueous sodium hydroxide solution was added to adjust the solution to pH9. The reaction mixture was stirred at 40° C. for 1.5 hrs and concentrated under reduced pressure. 5N Hydrochloric acid was added to acidify the solution (pH3) and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried (over anhydrous MgSO4). After concentration under reduced pressure, the precipitated solid was collected by filtration and washed with diisopropy ether to give the title compound (0.228 g) as a colorless powder with contamination.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07943770B2 |
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| 出典データセット | uspto-grants-2011_05 |
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| ORD ID | ord-fb0ae12249724eecae9fa971d3c4c9d9 |
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| 出典メモ | uspto-grants-2011_05 |
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