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Sodium Chloride → 4-Amino-1-dimethylamino-piperidine-4-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-(Dimethylamino)-4-piperidinone | HCID 56737782 | — |
| 溶媒 | Ammonia | HCID 222 | — |
| 生成物 | 4-Amino-1-dimethylamino-piperidine-4-carbonitrile | HCID 67225376 | — |
反応手順
6.3 g 1-Dimethylamino-piperidin-4-one (prepared as described in Journal of Medicinal & Pharmaceutical Chemistry, 4, 423-36; 1961) is dissolved in 135 ml aqueous ammonia (25%). To this solution 3.55 g ammonium chloride is added, then 4.34 g sodium cyanide. The reaction mixture is stirred at room temperature for 18 hours. Then the mixture is saturated with sodium chloride, and four times extracted with ethyl acetate. The organic layer is dried over sodium sulfate, and the solvent is evaporated, to yield 5.6 g 4-Amino-1-dimethylamino-piperidine-4-carbonitrile as a yellow oil. 1H-NMR (CDCl3): 2.95 ppm (m, 2H), 2.65 ppm (m, 2H), 2.40 ppm (s, 6H), 2.05 ppm (m, 2H), 1.80 ppm (m, 2H), 1.75 ppm (s, broad, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08703165B2 |
| 出典データセット | uspto-grants-2014_04 |
| ORD ID | ord-a2581c7f0c7e42fb9f16515d00b2bf06 |
| 出典メモ | uspto-grants-2014_04 |