関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | 2-Ethylhexyl bromide | HCID 86804 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Ethylheptanenitrile | HCID 137648 | — |
反応手順
A solution of KCN (3.8 g, 58 mmol) was stirred in DMF (150 mL) at room temperature. After the mixture was stirred for 2 h, a solution of 2-ethylhexylbromide (10 g, 52 mmol) in DMF (250 mL) was added dropwise at the same temperature. After stirring for 12 h at room temperature, the reaction mixture was concentrated by evaporation in vacuo. The crude product was diluted with water (100 mL) and diethyl ether (100 mL). The organic layer was separated and the aqueous layer was extracted with diethyl ether. The combined organic layers were subsequently washed with NaOH-solution (2.5 M), saturated bicarbonate solution and brine, dried over MgSO4 and concentrated by evaporation in vacuo. The resulting brown oil was purified by vacuum distillation (45° C., 10−2 mbar) to afford a clearly yellow oil (VI). (3.2 g, 44%). 1H-NMR (CDCl3): δ=2.82-2.69 (m, 2H), 2.22-2.15 (m, 1H), 1.55-1.00 (m, 11H), 0.83-0.68 (m, 3H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08329923B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-3250d223efde46b89d9713e034b23204 |
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| 出典メモ | uspto-grants-2012_12 |
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