関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | 3-Bromo-2-fluorobenzyl Alcohol | HCID 26985646 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | {2-Fluoro-3-[(trimethylsilyl)ethynyl]phenyl}methanol | HCID 86686224 | — |
反応手順
Under argon atmosphere, ethynyl(trimethyl)silane (9.0 ml) was mixed with triethylamine (50 ml), and (3-bromo-2-fluorophenyl)methanol, bis(triphenylphosphine)palladium chloride (II) (1.54 g), and copper iodide (420 mg) were added thereto, followed by stirring at 90° C. overnight. The reaction mixture was cooled to room temperature, and EtOAc was added thereto, followed by filtering using Celite as a filtration adjuvant. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/EtOAc) to obtain {2-fluoro-3-[(trimethylsilyl)ethynyl]phenyl}methanol (4.88 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09051283B2 |
|---|
| 出典データセット | uspto-grants-2015_06 |
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| ORD ID | ord-f2d73a44833f4b15956bc28d9ed61013 |
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| 出典メモ | uspto-grants-2015_06 |
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