関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium fluoride | HCID 25953 | — |
| 反応物 | (4-Chloro-2-methylphenyl)boronic acid | HCID 5017600 | — |
| 反応物 | 2-(5-Bromo-2-ethylphenyl)-4,4-dimethylcyclohexane-1,3-dione | HCID 66870121 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 2-(4'-Chloro-4-ethyl-2'-methylbiphen-3-yl)-4,4-dimethyl-cyclohexane-1,3-dione | HCID 123715133 | — |
反応手順
A mixture of 2-(5-bromo-2-ethylphenyl)-4,4-dimethylcyclohexane-1,3-dione (0.194 g, 0.6 mmol), 2-methyl-4-chloro-phenylboronic acid (0.153 g, 0.9 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (complex with dichloromethane 1:1) (80 mg, 0.098 mmol) and cesium fluoride (0.608 g, 4 mmol) are stirred together in 1,2-dimethoxyethane (4 ml) and the reaction mixture is heated at 80° C. overnight. The warm reaction mixture is filtered, washing the filter cake with 9:1 dichloromethane:methanol. The mixture is concentrated under reduced pressure and the residue is purified by column chromatography on silica gel to give 2-(4′-chloro-4-ethyl-2′-methylbiphen-3-yl)-4,4-dimethyl-cyclohexane-1,3-dione.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08741806B2 |
|---|
| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-2b6c5141eef649918800f0a6fff9105f |
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| 出典メモ | uspto-grants-2014_06 |
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