関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium amide | HCID 24533 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Chloro-1,1-diethoxypropane | HCID 96217 | — |
| 反応物 | 3-Methyl-2-(2-methylphenyl)butanenitrile | HCID 14245130 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 5,5-Diethoxy-2-isopropyl-2-(2-methylphenyl) valeronitrile | HCID 14245140 | — |
反応手順
The alkylation of 2-(2-methylphenyl)-3-methylbutyronitrile of Formula II: ##STR3## with 3,3-diethoxypropylchloride is carried out conveniently in an inert organic solvent in the presence of an alkaline condensing agent. Suitable inert organic solvents are aromatic hydrocarbons, e.g. benzene, toluene or commercial xylene, tertiary amides, e.g. dimethylformamide, or higher-boiling aliphatic ethers, e.g. ethyleneglycol dimethylether. Preferable alkaline condensing agent is sodium hydride or sodium amide. The reaction is advantageously effected by dropping a toluenic sodium amide suspension to a boiling solution of the above reactants in anhydrous toluene and refluxing the mixture for a period of 4 to 10 hours. The so formed acetal, 5,5-diethoxy-2-isopropyl-2-(2-methylphenyl) valeronitrile of Formula III: ##STR4## is isolated on cooling the mixture by short agitation with water, separation of the toluenic phase and evaporation of the solvent. The obtained crude product is purified by distillation under reduced pressure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04847403 |
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| 出典データセット | uspto-grants-1989_07 |
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| ORD ID | ord-0e189ea67b774e1c8e29061ef379abed |
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| 出典メモ | uspto-grants-1989_07 |
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