関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 4-Cyclopropylcarbonylphenylacetonitrile | HCID 15512831 | — |
| 反応物 | Potassium butoxide | HCID 23699084 | — |
| 生成物 | 4-(Cyclopropylcarbonyl)-alpha,alpha-dimethylbenzeneacetonitrile | HCID 23499845 | — |
反応手順
4-(Cyclopropylcarbonyl)phenylacetonitrile, 15.5 g [JOC, 1973,16, 487] and methyl iodide, 15.5 ml, are dissolved in 75 ml THF. The mixture is cooled to −10° C. and a solution of potassium butoxide (24.5 g) in THF (75 ml) is added so that the temperature of the reaction is kept below 5° C. After 0.5 h more, HPLC shows the reaction to be complete. 200 ml 2M HCI is added followed by 200 ml toluene. The organics are washed with 100 ml 10%. sodium sulphite solution then 100 ml satd sodium chloride solution. The THF is removed and the toluene treated with 5 g silica to remove colour. The toluene is removed and the product crystallises. Yield, 19 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176318B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-393840dc2e754777826692e274af5201 |
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| 出典メモ | uspto-grants-2007_02 |
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