関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-Ethylhexanoyl chloride | HCID 79103 | — |
| 反応物 | 2-(2'-Chlorophenyl)-5,5-dimethyl-1,3-cyclohexanedione | HCID 12876597 | — |
| 生成物 | 3-(2'-Ethylhexanoyloxy)-2-(2'-chlorophenyl)-5,5-dimethyl-2-cyclohexenone | HCID 13279765 | 82% |
反応手順
A solution of 1.009 (3.99 mmol) of 2-(2'-chlorophenyl)-5,5-dimethyl-1,3-cyclohexanedione and 0.03 g (8.0 mmol) of pyridine was cooled in an ice bath and stirred under N2. The 2-ethylhexanoyl chloride (0.69 g, 4.25 mmol) was added, the mixture was then allowed to warm to room temperature, stirred at room temperature for one hour and refluxed for one hour. The solvent was removed under reduced pressure and the residue taken up in ether and water. The ether was washed three times with 0.25N NaOH, three times with 10% HCl and with water. The ether was dried over anhydrous MgSO4 and decanted to give 1.23 g (82%) of 3-(2'-ethylhexanoyloxy)-2-(2'-chlorophenyl)-5,5-dimethyl-2-cyclohexenone as a clear colorless oil which was homogeneous by thin layer chromatography.
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-49bc1db3194845758af75f7d68b40fdd |
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| 出典メモ | uspto-grants-1986_09 |
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