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Potassium Hydroxide → 1-(1-((tert-butoxy)carbonyl)piperidin-4-yl)-1H-pyrazole-4-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Tert-butyl 4-(4-(ethoxycarbonyl)-1H-pyrazol-1-YL)piperidine-1-carboxylate | HCID 45926154 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(1-((tert-butoxy)carbonyl)piperidin-4-yl)-1H-pyrazole-4-carboxylic acid | HCID 53485897 | 82% |
反応手順
tert-Butyl 4-(4-(ethoxycarbonyl)-1H-pyrazol-1-yl)piperidine-1-carboxylate described in Production Example 13-2 (2.11 g, 6.53 mmol) was dissolved in methanol (60 mL), then potassium hydroxide (1.46 g, 26.1 mmol) dissolved in water (16 mL) was added, and then the mixture was stirred for 27 hours. The reaction mixture was concentrated under vacuum and diethyl ether was added for partition. Ethyl acetate was added to the aqueous layer for dilution, then a 5% aqueous potassium hydrogensulfate solution was added for acidification, and the mixture was extracted with ethyl acetate twice. The combined organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was evaporated to obtain the title compound (1.58 g, 82%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08933099B2 |
| 出典データセット | uspto-grants-2015_01 |
| ORD ID | ord-883a07d1c3fe4d91b9caad0dafa139ef |
| 出典メモ | uspto-grants-2015_01 |