関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Chloro-4-fluorobenzonitrile | HCID 109000 | — |
| 反応物 | 4-fluoro-L-phenylalanine | HCID 716312 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-(3-chloro-4-cyanophenyl)-4-fluorophenylalanine | HCID 67105225 | 100.1% |
反応手順
To a solution of 2-chloro-4-fluorobenzonitrile (1.8 g) in dimethyl sulfoxide (30 mL) were added 4-fluorophenylalanine (2.54 g) and cesium carbonate (4.90 g), and the mixture was stirred at 90° C. overnight. After allowing to room temperature, ethyl acetate was added, and the mixture was extracted twice with saturated aqueous sodium hydrogen carbonate solution. The aqueous layers were combined, and acidified with citric acid, and the mixture was extracted twice with ethyl acetate. The organic layers were combined, washed with saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give the title compound as a brown oil (yield: 3.69 g, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07834051B2 |
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| 出典データセット | uspto-grants-2010_11 |
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| ORD ID | ord-0b651756850d43d993669bcd544abd6d |
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| 出典メモ | uspto-grants-2010_11 |
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