関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Bromosalicylic acid | HCID 6972 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-Chloro-4-fluorophenylboronic Acid (contains varying amounts of Anhydride) | HCID 2734660 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 3'-Chloro-4'-fluoro-4-hydroxy-biphenyl-3-carboxylic acid | HCID 21921317 | 43.8% |
反応手順
3-Chloro-4-fluoro-phenylboronic acid (3.2 g, 18.4 mmol), 5-bromo-2-hydroxy-benzoic acid (4.0 g, 18.4 mmol), and Pd (PPh3)4 (1.67 g, 1.84 mmol) were dissolved in 250 mL of DME, a 1 M Na2CO3 solution (46 mL, 46.0 mmol) added and the mixture heated to 80° C. for 20 h. The reaction mixture was filtered, partially evaporated and EtOAc (200 mL) and 1 N HCl (100 mL) added. The organic layer washed with 1N HCl and saturated sodium bicarbonate, dried over sodium sulfate, and evaporated. The crude material was filtered through a silica plug (THF) to give 3′-chloro-4′-fluoro-4-hydroxy-biphenyl-3-carboxylic acid (2.15 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07459472B2 |
|---|
| 出典データセット | uspto-grants-2008_12 |
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| ORD ID | ord-90c5c581e3844ef390a161f7f73dad68 |
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| 出典メモ | uspto-grants-2008_12 |
|---|
