関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Levofloxacin | HCID 149096 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | Levofloxacin Hydrate | HCID 3033924 | 108.9% |
反応手順
25 g of wet levofloxacin crude (about 22.17 g or dry levofloxacin) was put in suspension in 225 mL of mixture ACN:H2O (99:1) under nitrogen atmosphere. The mixture was heated to reflux during 1 hour and then filtrated under vacuum with Hyflow when still hot. Then the solution was heated again to reflux and cooled to 0° C. over a period of 1 hour. The precipitate was filtrated under vacuum, washed with ACN:H2O (2×12 mL) and dried in a vacuum oven to give 18.6 g (84%) of purified levofloxacin hemihydrate. The purified levofloxacin hemihydrate contained approximately one-third less desmethyl levofloxacin than in the crude sample.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425628B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-3a561d923a7b4eb78c307814fe5df863 |
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| 出典メモ | uspto-grants-2008_09 |
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