関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl 6-(2',4'-dimethylphenyl)-6-cyano-3,3-dimethylhexanoate | HCID 13688117 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(2,4-Dimethylphenyl)-5,5-dimethylcyclohexane-1,3-dione | HCID 12556345 | 32% |
反応手順
A one-neck round bottom flask was charged with 52.50 g (0.17 mol) of ethyl 6-(2',4'-dimethylphenyl)-6-cyano-3,3-dimethylhexanoate, 250 ml of concentrated hydrochloric acid, 250 ml of glacial acetic acid, and 100 ml of water. The reaction mixture was stirred and refluxed for 48 hours. After 12 hours and 24 hrs. of refluxing, an additional 100 ml of conc. HCl and 100 ml glacial HOAC were added. After 48 hours, the mixture was stripped to dryness under reduced pressure. To the residue were added 150 ml of water and 150 ml of ethyl ether, and the mixture shaken vigorously. A white, crystalline precipitate formed, and this was removed by suction filtration to give 13.20 g (32%) of 2-(2',4'-Dimethylphenyl)-5,5-dimethyl-1,3-cyclohexanedione as a white, crystalline solid, m.p. 167°-168.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04613617 |
|---|
| 出典データセット | uspto-grants-1986_09 |
|---|
| ORD ID | ord-6dedfb60a769493fb93ce38218265fab |
|---|
| 出典メモ | uspto-grants-1986_09 |
|---|