関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Ethylhexanoyl chloride | HCID 79103 | — |
| 反応物 | 2-(2',5'-Dimethylphenyl)-5,5-dimethyl-1,3-cyclohexanedione | HCID 12876602 | — |
| 触媒 | Dicyclohexano-18-crown-6 | HCID 85955 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3-(2-Ethylhexanoyloxy)-5,5-dimethyl-2-(2',5'-dimethylphenyl)-2-cyclohexenone | HCID 20206510 | 92% |
反応手順
A suspension of 1.50 g (6.14 mmol) of 2-(2',5'-dimethylphenyl)-5,5-dimethyl-1,3-cyclohexanedione in 15 ml of dry benzene was prepared and 0.49 g (7.37 mmol) of 85% powered potassium hydroxide was added, followed by 1 drop of dicyclohexyl-18-crown-6-ether. After stirring for 30 minutes, 1.20 (7.37 mmol) of 2-ethylhexanoyl chloride was added, and the reaction mixture refluxed for 12 hrs. The reaction mixture was cooled to room temperature, taken up in 150 ml ether and 50 ml of water, washed three times with 0.25N NaOH, two times with water, two times with 6N HCl, and one more with water. The ether solution was dried and stripped to leave 2.10 g (92% yield) of 3-(2-ethylhexanoyloxy)-5,5-dimethyl-2-(2',5'-dimethylphenyl)-2-cyclohexenone as a clear, colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04613617 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-34b48e88f482444b8bff393b770af19f |
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| 出典メモ | uspto-grants-1986_09 |
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