関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | 4-Fluorobenzaldehyde | HCID 68023 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(4-fluorophenyl)-2-(N,N-dimethylamino)acetonitrile | HCID 11309856 | 90.5% |
反応手順
Into a 1 l four-necked flask equipped with a thermometer, a stirrer and a dropping funnel, 49.6 g (0.4 mol) of 4-fluorobenzaldehyde and 480 ml of acetonitrile were charged, and a solution comprising 29.4 g (0.64 mol) of sodium cyanide, 81.6 g (1 mol) of dimethylamine hydrochloride and 200 ml of water, was dropwise added over a period of 15 minutes at from 20 to 30° C. with stirring, and then reacted at the same temperature for 18 hours. After completion of the reaction, the mixture was subjected to liquid separation. The organic layer was separated, and acetonitrile was distilled off. The residue was extracted with 400 ml of ethyl acetate, washed with a 5% sodium hydrogen carbonate aqueous solution and water, and then dried over anhydrous sodium sulfate. Ethyl acetate was distilled off, and the obtained oily substance was distilled under reduced pressure to obtain 64.5 g (yield: 90.5%) of the desired compound (boiling point: 100-101° C./1 KPa). The NMR spectrum data thereof are as follows.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06956132B2 |
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| 出典データセット | uspto-grants-2005_10 |
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| ORD ID | ord-103d802ac778452fa9db922f353ede9e |
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| 出典メモ | uspto-grants-2005_10 |
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