関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | Ethyl 1-formylcyclopropanecarboxylate | HCID 9964122 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(1-Benzylamino-1-cyanomethyl)-1-ethoxycarbonylcyclopropane | HCID 15391046 | 87.1% |
反応手順
An eggplant type flask was charged with 131 mg of potassium cyanide and 539 mg of benzylamine, and the contents were dispersed in 1 ml of water. Thereto was added dropwise 146 mg of ethyl 1-formylcyclopropane-1-carboxylate dissolved in 2 ml of ethanol at room temperature, followed by dropwise addition of 0.2 ml of concentrated hydrochloric acid. The reaction solution was stirred for 2.5 hours at 50° C. After confirming completion of the reaction, the reaction solution was mixed with ice water and extracted with ethyl acetate. Next, the resulting organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and, after removing insoluble matter by filtration, concentrated under a reduced pressure. Thereafter, the resulting residue was subjected to a silica gel column chromatography (hexane:ethyl acetate=5:1) to obtain 231 mg (87%) of the title compound in the form of colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06218548B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-58070d59708343a6b8b526198dd53907 |
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| 出典メモ | uspto-grants-2001_04 |
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