関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Bromo-2,6-dichlorobenzene | HCID 29568 | — |
| 反応物 | 5-Fluoro-2-methoxyphenylboronic acid | HCID 2782673 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water 1,2-dimethoxyethane | HCID 18180031 | — |
| 生成物 | 2',6'-Dichloro-5-fluoro-2-methoxybiphenyl | HCID 58646955 | 87% |
反応手順
To a solution of 2,6-dichlorobromobenzene (3.5 g, 15.7 mmol) and sodium hydroxide (3.14 g, 78.5 mmol) in DME-water (2:1) was added 5-fluoro-2-methoxybenzene boronic acid (4.0 g, 23.5 mmol) at 90° C., followed by tetrakis(triphenylphosphine)palladium (0) (0.9 g, 0.78 mmol). The reaction mixture was heated at 90° C. overnight and cooled to room temperature. The mixture was extracted with methylene chloride and washed with water. The organic solvent was removed under vacuum. Chromatography with 5% ethyl acetate in hexanes afforded 2.62 g (87%) of 2′,6′-dichloro-5-fluoro-2-methoxybiphenyl as a colorless oil. MS (EI) m/z 270 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07365095B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-2542c6f5ef0c48458405b2ca8702a00d |
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| 出典メモ | uspto-grants-2008_04 |
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