関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzoic acid, 4-fluoro-, ethyl ester | HCID 67976 | — |
| 反応物 | 1-Cyclobutylpiperazine | HCID 4738602 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Ethyl 4-(4-cyclobutylpiperazin-1-yl)benzoate | HCID 57440408 | 33% |
反応手順
Ethyl 4-fluorobenzoate (0.753 g, 4.48 mmol) was added to a solution of 1-cyclobutylpiperazine (0.571 g, 4.07 mmol) and potassium carbonate (0.563 g, 4.07 mmol) in DMSO (8 mL) under nitrogen. The resulting solution was stirred at 100° C. for 18 h and evaporated to dryness. The residue was triturated with diethyl ether, filtered, and evaporated and the crude product was purified by silica column chromatography, eluting with a gradient of 0 to 2.5% 2.5N MeOH in DCM. Pure fractions were evaporated to dryness to afford ethyl 4-(4-cyclobutylpiperazin-1-yl)benzoate (0.387 g, 32.9%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737149B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-4a50fabbb59a43498f3a1e1ac535a4bc |
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| 出典メモ | uspto-grants-2010_06 |
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