関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 4-Fluorothiophenol | HCID 67789 | — |
| 反応物 | 2-Chloro-5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)nicotinonitrile | HCID 10150677 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-(4-Chlorophenyl)-6-(2,4-dichlorophenyl)-2-(4-fluorophenylthio)nicotinonitrile | HCID 10311095 | — |
反応手順
An oven-dried round bottom flask was charged with 60.0 mg (0.152 mmol) of the product of Example 36 and Cs2CO3 (250.0 mg, 0.767 mmol), toluene (1.0 mL) and 4-fluorobenzene thiol (97.5 mg, 0.761 mmol) were added sequentially. The reaction was heated to 100° C. for 23 hours and then allowed to cool to room temperature at which point the reaction was filtered and concentrated. The residue was purified by preparative thin layer chromatography (20 cm×20 cm, 1000 μm, silica gel) eluting with 10:90 EtOAc-hexane affording a white solid). MS (electrospray) m/e 487 MH+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07271266B2 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-8914b0d84d26416787fa26fdeba3d078 |
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| 出典メモ | uspto-grants-2007_09 |
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