関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | 2-Cyclohexen-1-one, 3-phenyl- | HCID 82567 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Trimethylamine Hydrochloride | HCID 10313079 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Oxo-1-phenylcyclohexanecarbonitrile | HCID 12339122 | 92% |
反応手順
A mixture of 3-phenylcyclohex-2-enone (14.3 mmol), potassium cyanide (1.92 g) and trimethylamine hydrochloride (2.06 g, 21.5 mmol) in H2O (10 mL) and DMF (57 mL) was heated at 93° C. for 6 hr. After cooling down to room temperature, saturated sodium bicarbonate was added and the organic layer was separated. The aqueous layer was extracted with diethyl ether 3 times. The combined organic layers were washed with saturated sodium chloride solution, dried over magnesium sulfate, filtered and concentrated under vacuum to get 2.62 g of the crude 3-oxo-1-phenylcyclohexanecarbonitrile which was directly taken to the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07098203B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-252ad776d6b649efaee5e0abcd5fe44a |
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| 出典メモ | uspto-grants-2006_08 |
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