関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 3-Cyano-4-fluorophenylboronic acid | HCID 2757964 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 反応物 | 1-{[4-Bromo-5-(3-chlorophenyl)thiophen-2-yl]carbonyl}imidazolidin-4-one | HCID 58066740 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | HCID 46833796 | HCID 46833796 | — |
反応手順
Under argon, 61.0 mg (0.16 mmol) of the compound from Example 24A are provided in 3 ml of 1,2-dimethoxyethane, and 26.1 mg (0.16 mmol) of 3-cyano-4-fluorophenylboronic acid, 155 mg (0.47 mmol) of cesium carbonate, 5.3 mg (0.01 mmol) of dicyclohexyl[2′,4′,6′-tri(propan-2-yl)biphenyl-2-yl]phosphane and 1.1 mg (0.005 mmol) of palladium(II) acetate are added. The mixture is heated in a closed glass vessel at 100° C. under microwave irradiation for 30 minutes. The reaction mixture is purified by preparative HPLC (RP18 column; eluent: acetonitrile/water gradient). 23.0 mg (34% of theory) of the title compound are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08546438B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-80d990ba71a64f73bb1bd84f1f8c4f67 |
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| 出典メモ | uspto-grants-2013_10 |
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