関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Chloro-1-fluoro-4-nitrobenzene | HCID 67688 | — |
| 反応物 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Tert-butyl 4-(2-chloro-4-nitrophenyl)piperazine-1-carboxylate | HCID 18783805 | 64.7% |
反応手順
A mixture of 3-chloro-4-fluoronitrobenzene (5 g, 27.1 mmol), 1-piperazinecarboxylic acid t-butyl ester (5 g, 26.8 mmol) and dimethylformamide (10 mL) was stirred for 3 hours and 30 minutes at an external temperature of 130° C. After adding water to the air-cooled reaction mixture, extraction was performed 3 times with chloroform. The organic layers were washed with brine and dried over anhydrous magnesium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel colurn chromatography (ethyl acetate/heptane) to give 5.93 g of the title compound as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425554B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-293bca3bde1e4e4ab038e84ec05c91b5 |
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| 出典メモ | uspto-grants-2008_09 |
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