関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| 反応物 | 2-Butenal, 2-ethyl- | HCID 5362897 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (E,E)-4-ethyl-2,4-hexadienenitrile | HCID 14329794 | 41% |
反応手順
To a mixture of sodium hydride (60% in oil, 7.5 g) and dry benzene (200 ml) was added dropwise diethyl cyanomethylphosphonate (30 g) with stirring at 0° C. under dry nitrogen atmosphere. After stirring for 60 minutes at room temperature, a solution of (E)-2-ethyl-2-butenal (16.6 g) in dry benzene was added thereto at 0° C. with stirring. The resulting mixture was allowed to stand at room temperature for 60 minutes and diluted with water and then extracted with ethyl acetate. The extract was washed successively with water and brine, and then dried over magnesium sulfate. Removal of the solvent gave an oil which was purified by distillation under reduced pressure to give (E,E)-4-ethyl-2,4-hexadienenitrile (8.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04767768 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-92c75c2f96ad4384a5b901ce45dfdb1d |
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| 出典メモ | uspto-grants-1988_08 |
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