関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Methyl 5-cyano-5-(4-fluorophenyl)-2-oxocyclohexanecarboxylate | HCID 12230235 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile | HCID 91805 | 67% |
反応手順
A reaction mixture consisting of 33.9 gm. (0.123 mole) of 2-carbomethoxy-4-cyano-4-(p-fluorophenyl)cyclohexanone (prepared in Part B, above), 900 ml. glacial acetic acid, and 450 ml. 10% aqueous sulfuric acid is heated with stirring on a steam bath for 24 hours. After allowing the reaction mixture to cool, it is diluted with 2000 ml. water and extracted thoroughly with benzene. The benzene extracts are combined and washed successively with water, with aqueous sodium bicarbonate, and finally with brine. The benzene is then removed by evaporation under reduced pressure, and the solid residue thus obtained is recrystallized from diethyl ether to afford 16.23 gm. (67% yield) of 4-cyano-4-(p-fluorophenyl)cyclohexanone having a melting point at 84° to 88° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04065573 |
|---|
| 出典データセット | uspto-grants-1977_12 |
|---|
| ORD ID | ord-4d7e11105d8f47409fb7e8b110241c34 |
|---|
| 出典メモ | uspto-grants-1977_12 |
|---|