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Trimethylsilylacetylene → ((4-Chloro-2-fluorophenyl)ethynyl)trimethylsilane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | 4-Chloro-2-fluoro-1-iodobenzene | HCID 2736562 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | ((4-Chloro-2-fluorophenyl)ethynyl)trimethylsilane | HCID 90019293 | 56.5% |
反応手順
To a solution of 4-chloro-2-fluoro-1-iodobenzene (2.0 g, 7.8 mmol) in DMSO (10 mL) was added ethynyl(trimethyl)silane (1.14 g, 11.0 mmol), copper iodide (0.029 g, 0.15 mmol), bis(triphenylphosphine) palladium(II) chloride (0.218 g, 0.3 mmol) and TEA (1 mL). The reaction mass was stirred at RT for 4-5 h. The reaction mass quenched in water, passed through celite bed and extracted with ethyl acetate and concentrated to afford 1.0 g of desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09439890B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-649418e8072746319213417db71ea5ca |
| 出典メモ | uspto-grants-2016_09 |