関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Butylamine | HCID 8007 | — |
| 反応物 | Rosuvastatin n-butylamide | HCID 86699893 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Rosuvastatin | HCID 446157 | 102.4% |
反応手順
An autoclave having 800 cm3 is charged with 16.1 g (0.03 mol) rosuvastatin n-butylamide, 644 cm3 of water and 43.9 g (63.3 cm3; 0.60 mol) of n-butylamine. The reaction mixture is stirred at 120° C. for 24 hours, allowed to cool, diluted with 2-propanol at room temperature and evaporated in vacuo. The residue is boiled in ethylacetate, and while stirring, allowed to cool to room temperature. The crystals are filtered. Thus 14.8 g (89%) of rosuvastatin NBA salt are obtained. The crude salt is stirred in ethylacetate at room temperature, filtered, washed and dried. Thus dried product is boiled in ethylacetate, thereafter stirred in the same solvent at room temperature, filtered, washed and dried. Yield 9.32 g (56%) of rosuvastatin NBA salt, having purity (as determined by HPLC) exceeding 99.5%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09040696B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-b9f9d6028af0454a98728bba3a69a714 |
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| 出典メモ | uspto-grants-2015_05 |
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