関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-(Trifluoromethyl)phenylboronic acid | HCID 2734388 | — |
| 反応物 | 3-Bromothiophene-2-carboxaldehyde | HCID 2797079 | — |
| 触媒 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 4-(4-Trifluoromethylphenyl)thiophene-2-carbaldehyde | HCID 11736954 | — |
反応手順
To a solution of 3-bromothiophene-2-carboxaldehyde (2.0 g) and 3-trifluoromethylbenzene boronic acid (2.19 g) in ethylene glycol dimethyl ether (100 ml) was added sodium carbonate (2.9 g), tetrakis(triphenylphosphine) palladium (0) (0.12 g) and water (50 ml). The mixture was heated to 90° C. under nitrogen. After 18 hours the reaction was allowed to cool and was concentrated. The residue was partitioned between water and ethyl acetate; the organic solution was taken and was washed with brine and then dried (MgSO4) and concentrated. The crude material was purified by SPE (Si); the product eluted with neat chloroform to furnish the title compound as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091237B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-ffa3f6e62ec945dc861cc1427e46b8f0 |
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| 出典メモ | uspto-grants-2006_08 |
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