関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Atorvastatin | HCID 60823 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzathine | HCID 8793 | — |
| 生成物 | Atorvastatin | HCID 60823 | — |
| 生成物 | 3-Phenylpropane-1,2-diamine | HCID 413434 | — |
反応手順
The benzathine 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 N,N′-bis(phenylmethyl-1,2-ethanediamine (benzathine) was prepared by dissolving 220.64 mg (0.5 equivalents) in acetonitrile (80 mL) and water (20 mL). The stock solution of atorvastatin free acid was added to the counterion solution with stirring. After 2 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 benzathine 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-45777a62c3a540f0aec199c98e0a898a |
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| 出典メモ | uspto-grants-2014_09 |
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