関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Atorvastatin | HCID 60823 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Diethylamine | HCID 8021 | — |
| 生成物 | Atorvastatin | HCID 60823 | — |
| 生成物 | Atorvastatin diethylamine | HCID 11556397 | — |
反応手順
The diethylamine salt of atorvastatin (Form B) was synthesized by preparing a stock solution of the free acid of atorvastatin (U.S. Pat. No. 5,273,995) in acetonitrile (1 g in 40 mL of ACN). A solution of diethylamine was prepared by dissolving 132.33 mg (1.0 equivalents) in acetonitrile (20 mL). The stock solution of atorvastatin free acid was added to the counterion solution with stirring. Over time, an additional 40 mL of acetonitrile was added to prevent the formation of a gel. After 5 days of stirring at ambient temperature, the solids were isolated by vacuum filtration using a Buchner funnel fitted with a paper filter (#2 Whatman). The solids were rinsed with acetonitrile (75 mL) to afford atorvastatin diethylamine Form B. Note that this procedure is the same as above except that the sample was not oven dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822703B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-4d610403326443e2b8cd826b6f260619 |
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| 出典メモ | uspto-grants-2014_09 |
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