関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 4-Bromo-3-chlorotoluene | HCID 138789 | — |
| 反応物 | Ethyl 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate | HCID 2773962 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2'-Chloro-4'-methyl-biphenyl-2-carboxylic acid ethyl ester | HCID 59492677 | 126% |
反応手順
Under an argon atmosphere, 4-bromo-3-chlorotoluene (200 g), ethyl 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (376 g), toluene (1000 ml), water (1000 ml), tripotassium phosphate (412 g) and dichlorobis(triphenylphosphine)palladium(II) (14 g) were added to a reaction vessel and the mixture was stirred at 110° C. for 2 hr. The reaction mixture was cooled to room temperature. The insoluble material was filtered off, and washed with water (500 ml) and toluene (500 ml). The filtrate was partitioned in a separatory funnel. The organic layer was washed twice with water (1000 ml), dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure to give the title compound (337 g). The obtained residue was directly used for the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08871934B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-0d92cfa523014d60b4ddb2db0ade9306 |
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| 出典メモ | uspto-grants-2014_10 |
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