関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Dimethylpiperazine | HCID 66056 | — |
| 反応物 | Benzoic acid, 4-fluoro-, ethyl ester | HCID 67976 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Ethyl 4-(3,5-dimethylpiperazin-1-yl)benzoate | HCID 18425275 | 76% |
反応手順
2,6-Dimethylpiperazine(3.43 g, 30.00 mmol) was added to ethyl 4-fluorobenzoate (1.101 mL, 7.5 mmol), in DMSO (10 mL) warmed to 120° C. under nitrogen. The resulting solution was stirred at 120° C. for 20 h. The reaction mixture was cooled and the solvent was evaporated. The crude product was purified by silica column chromatography, eluting with 10% methanol in dichloromethane containing 1% 0.880 ammonia. Pure fractions were evaporated to dryness to afford ethyl 4-(3,5-dimethylpiperazin-1-yl)benzoate (1.490 g, 76%) as a colourless 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-04477e76365a42e9aa1f377a5189eaff |
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| 出典メモ | uspto-grants-2010_06 |
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