関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 反応物 | Methyl 3,4-difluorobenzoate | HCID 2775358 | — |
| 生成物 | Tert-butyl 4-(2-fluoro-4-(methoxycarbonyl)phenyl)piperazine-1-carboxylate | HCID 23117202 | 44.9% |
反応手順
Potassium carbonate (5.56 g, 40.3 mmol) and tert-butyl piperazine-1-carboxylate (6.92 g, 37.2 mmol) were combined; methyl 3,4-difluorobenzoate (5.33 g, 31.0 mmol) was added, and the reaction mixture was stirred at 90° C. for 1 d. The mixture was triturated with ethyl acetate (3×5 mL) and the combined organic extracts were filtered, concentrated down to about 5-10 mL, and subjected to flash column chromatography on silica gel (120 g SiO2, hexanes:ethyl acetate 1:0 to 4:1) to afford the title compound as a white solid (4.702 g, 13.90 mmol, 44.9% yield). ESI-MS: m/z 339 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08669249B2 |
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| 出典データセット | uspto-grants-2014_03 |
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| ORD ID | ord-21a007faa98940d7af2d37a68d5a5c5e |
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| 出典メモ | uspto-grants-2014_03 |
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