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Toluene → 1,4-Dioxaspiro[4.5]decane-8-carbonitrile, 8-(4-fluorophenyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile | HCID 91805 | — |
| 生成物 | 1,4-Dioxaspiro[4.5]decane-8-carbonitrile, 8-(4-fluorophenyl)- | HCID 12230242 | — |
反応手順
15 g of 1-(4-Fluoro-phenyl)-4-oxo-cyclohexanecarbonitrile (12) were dissolved in 500 mL of toluene, then 900 mg of p-toluene sulfonic acid were added and the reaction mixture was heated in a Dean-Stark apparatus for 6 h. The mixture was allowed to cool to room temperature and washed twice with saturated aqueous sodium bicarbonate solution and brine, dried over magnesium sulphate and evaporated to dryness to yield 17.9 g of the desired product. Rt=1.47 min (Method 5). Detected mass: 262.2 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541449B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-eb57cc6faa9a46448c8693c8bd34b229 |
| 出典メモ | uspto-grants-2013_09 |