関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Fluoro-4-(methoxycarbonyl)benzeneboronic acid | HCID 2782818 | — |
| 反応物 | 1-(3-Bromo-5-chloro-2-methoxy-4-methylphenyl)ethanone | HCID 86666759 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Sodium Carbonate | HCID 10340 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Methyl 3'-acetyl-5'-chloro-3-fluoro-2'-methoxy-6'-methylbiphenyl-4-carboxylate | HCID 86666801 | — |
反応手順
A mixture of 1-(3-bromo-5-chloro-2-methoxy-4-methylphenyl)ethanone (1.0 g, 3.6 mmol) and [3-fluoro-4-(methoxycarbonyl)phenyl]boronic acid (0.85 g, 4.3 mmol) in 1,4-dioxane (12 mL) and 10% sodium carbonate in water (5.73 mL, 5.40 mmol) was bubbled with N2 to degas. After tetrakis(triphenylphosphine)palladium(0) (166 mg, 0.144 mmol) was added, the mixture was bubbled with N2 for 5 min. more and heated at 100° C. overnight. The mixture was cooled to room temperature and diluted with ethyl acetate. The layers were separated and the aq. layer was extracted with more ethyl acetate. The combined extracts were washed with brine, dried over Na2SO4, filtered, and concentrated to give crude product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09096600B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-b74237beef2345269d14478eb90f3d6b |
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| 出典メモ | uspto-grants-2015_08 |
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