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Sodium Carbonate → 2'-Fluoro-2,3-dimethoxybiphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1-Bromo-2-fluorobenzene | HCID 61259 | — |
| 反応物 | 2,3-Dimethoxybenzeneboronic acid | HCID 5156491 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 2'-Fluoro-2,3-dimethoxybiphenyl | HCID 57264076 | 85% |
反応手順
In the atmosphere of argon, 18.2 g of 2,3-dimethoxyphenylboronic acid, 17.5 g of 2-fluorobromobenzene, 2.31 g of tetrakistriphenylphosphine palladium (0), 300 mL of 1,2-dimethoxyethane and 150 mL of an aqueous 2M sodium carbonate solution were placed in a flask. The resulting mixture was stirred with heating under reflux for 8 hours. After cooling to room temperature, an aqueous phase was removed, and an organic phase was washed with saturated saline. The organic phase was dried with magnesium sulfate and then concentrated. Residues were purified by silica gel column chromatography, whereby 19.7 g of (yield 85%) of 2′-fluoro-2,3-dimethoxybiphenyl was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08629430B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-7945c7618e4a4cf3a4fa1638c02cf341 |
| 出典メモ | uspto-grants-2014_01 |