関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride | HCID 68776288 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine | HCID 68776289 | 56.8% |
反応手順
A 4 N solution (50 ml) of hydrogen chloride in ethyl acetate was added to a solution of tert-butyl 4-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxylate (4.20 g, 11.0 mmol) in ethyl acetate (100 ml), and the mixture was stirred at room temperature for 14 hours. Hexane was added to the reaction mixture, and crystals were collected by filtration to give 1-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride. The hydrochloride was dissolved in water, neutralized with a 1 N sodium hydroxide aqueous solution, and extracted with chloroform. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give 1.76 g (56.8%) of the desired product as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07851473B2 |
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| 出典データセット | uspto-grants-2010_12 |
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| ORD ID | ord-a0dc484bb6a1418eaf18f6d2c2bc8459 |
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| 出典メモ | uspto-grants-2010_12 |
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