関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 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 | 98.4% |
反応手順
Into a 1 l four-necked flask equipped with a thermometer, a stirrer and a dropping funnel, 144.5 g (1.6 mol) of a 50.7% dimethylamine aqueous solution and 118.5 g of water were charged, and 159.4 g (0.38 mol) of a 25% of sulfuric acid aqueous solution was dropwise added over a period of 15 minutes at a temperature of not higher than 20° C. with stirring. Then, 67.4 g (1.38 mol) of sodium cyanide was introduced. Then, 155.1 g (1.25 mol) of 4-fluorobenzaldehyde was dropwise added over a period of 20 minutes at from 20 to 30° C. Thereafter, the reaction was carried out at 50° C. for 4 hours. After completion of the reaction, the reaction mixture was subjected to liquid separation. The organic layer was separated and washed with 500 ml of water of 50° C. to obtain 222.8 g (yield: 98.4%) of the desired compound having a purity of 98.4% (by GC analysis).
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-812e62ea85a7484cbe5e45f6336653c1 |
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| 出典メモ | uspto-grants-2005_10 |
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