関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Succinic anhydride | HCID 7922 | — |
| 反応物 | 8-Fluorociprofloxacin | HCID 122848 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 11762141 | HCID 11762141 | 55.7% |
反応手順
3.5 g (0.01 mol) of 1-cyclopropyl-6,8-difluoro-7-(piperazin-1-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid are dissolved in a mixture of 0.4 g of sodium hydroxide in 20 ml of water, and a solution of 1 g of succinic anhydride in 10 ml of dioxane, and a solution of 0.4 g of sodium hydroxide in 10 ml of water, are simultaneously added dropwise at 20° C. After standing for 12 hours, the mixture is adjusted to pH 5 with 2N hydrochloric acid, and the precipitate is filtered off under suction, washed with water, heated with methanol, filtered off under suction and dried. 2.5 g of 7-[4-(3-carboxypropionyl)-piperazin-1-yl]-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid having a decomposition temperature of 217°-219° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04556658 |
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| 出典データセット | uspto-grants-1985_12 |
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| ORD ID | ord-5a2ec8a831924e50b59e725c2cc097ae |
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| 出典メモ | uspto-grants-1985_12 |
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