関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Hydride | HCID 166653 | — |
| 反応物 | Butanoic acid, 2-ethyl-2-methyl-, methyl ester | HCID 521437 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Hexanenitrile, 4-ethyl-4-methyl-3-oxo- | HCID 159096 | — |
反応手順
To a suspension of 96 g. of sodium hydride, as a 50% dispersion in mineral oil, in 300 ml. of dry tetrahydrofuran was added, with stirring, 63 g. of acetonitrile and 114 g. of methyl 2-ethyl-2-methylbutyrate. The mixture was then heated gently to 60°-65° and allowed to reflux gently at that temperature overnight. It was then cooled to ice bath temperature, and 2-ml. portions of ethanol were added to decompose the remaining hydride. When the mixture did not foam on further ethanol addition, the mixture was evaporated under vacuum to dryness, and the residue was dumped into 4 liters of water. The aqueous mixture was extracted with hexane to remove the mineral oil, and it was then made acid to pH 2 and was extracted with two 1-liter portions of diethyl ether. The ether was dried over magnesium sulfate and evaporated under vacuum to obtain 122 g. of the desired acetonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04411753 |
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| 出典データセット | uspto-grants-1983_10 |
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| ORD ID | ord-1c4edb83a7a4493689aab3ae7451f2f1 |
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| 出典メモ | uspto-grants-1983_10 |
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