関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ketoprofen | HCID 3825 | — |
| 反応物 | (S)-3-Methyl-2-phenylbutylamine | HCID 10176271 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | Dexketoprofen | HCID 667550 | 60.7% |
反応手順
(±)-2-(3-Benzoylphenyl)propionic acid (12.7 g, 50 mmol) was added to methyl ethyl ketone (hereinafter abbreviated to "MEK") (70 ml) and dissolved with heating. Then, (S)-(+)-3-methyl-2-phenylbutylamine (4.9 g, 30 mmol) was added dropwise with stirring. After completing the addition, the reaction solution was stirred at 35°C. to 40°C. for one hour and then at room temperature for 4 hours, and finally maintained at 10°C. for 3 hours. The crystal precipitated was filtered, and the filter cake was washed with cold MEK (35 ml) and dried to give a diastereomer salt (7.72 g) of (S)-(+)-2-(3-benzoylphenyl) propionic acid with (S)-(+)-3-methyl-2-phenylbutylamine. The yield of the product based on (S)-(+)-2-(3-benzoylphenyl) propionic acid contained in the starting material was 74%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05852209 |
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| 出典データセット | uspto-grants-1998_12 |
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| ORD ID | ord-9ca4ba25cea346afb2de01712e165811 |
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| 出典メモ | uspto-grants-1998_12 |
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