関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | 3-(2,4-Dichloro-pyrimidin-5-yl)-2-phenyl-propionic acid methyl ester | HCID 21044322 | — |
| 生成物 | 3-(2,4-Diphenylamino-pyrimidin-5-yl)-2-phenyl-propionic acid methyl ester | HCID 21044325 | — |
反応手順
The mixture of 3-(2,4-dichloro-pyrimidin-5-yl)-2-phenyl-propionic acid methyl ester (0.31 g, 1.0 mmol) (from Example 5a supra) and aniline (3.0 mL) (Aldrich) was heated at 120° C. for 1 hour. The reaction mixture was washed with hexanes (50 mL×3) and the supernatant was decanted off after each time. The residue was then dissolved in ethyl acetate (100 mL) and successively washed with saturated aqueous ammonium chloride solution (30 mL), water (30 mL) and brine (30 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The crude product was purified by flash column chromatography (silica gel) to give 3-(2,4-diphenylamino-pyrimidin-5-yl)-2-phenyl-propionic acid methyl ester as a white amorphous solid. (Yield 0.35 g, 82.3%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098332B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-52bce4e4c8a344a39a7507d5991567b3 |
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| 出典メモ | uspto-grants-2006_08 |
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