関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | Benzene, 1-iodo-3-(trifluoromethyl)- | HCID 67868 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-[(Trimethylsilyl)ethynyl]-3-(trifluoromethyl)benzene | HCID 4281885 | 57.3% |
反応手順
To a solution of 1-iodo-3-(trifluoromethyl)benzene (1.0 g, 3.6 mmol) in ethyl acetate (20 mL) was added ethynyl(trimethyl)silane (0.540 g, 5.5 mmol), copper iodide (0.042 g, 0.22 mmol), bis(triphenylphosphine) palladium(II) chloride (0.129 g, 0.18 mmol) and TEA (2.2 mL, 14.7 mmol). The reaction mass stirred at 50-60° C. for 24 h. The reaction mass was quenched in water, extracted with ethyl acetate and concentrated to afford 0.500 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 0.26 (s, 9H), 7.44 (t, J=7.8 Hz, 1H), 7.55 (d, J=7.8 Hz, 1H), 7.62 (d, J=7.2 Hz, 1H), 7.72 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09439890B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-db091dd852e94dac8377a99e56e3cd33 |
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| 出典メモ | uspto-grants-2016_09 |
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