関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-Chloro-2-fluoro-1-nitrobenzene | HCID 69691 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(5-Chloro-2-nitrophenyl)piperidine | HCID 3096079 | 97% |
反応手順
To a cooled (0° C.) solution of 1.75 g (10.0 mmol) of 4-chloro-2-fluoronitrobenzene in 15 mL of EtOH was added 2.97 mL (30.0 mmol) of piperidine dropwise over 5 min. The solution stirred at 0° C. for 10 min and then at 23° C. for 30 min. The mixture was poured into water (225 mL) and extracted with EtOAc (2×30 mL). The combined extracts were washed with saturated aq NaHCO3 and brine (30 mL each) and then dried (Na2SO4). Concentration afforded 2.33 g (97%) of the title compound as an orange oil which crystallized on standing: Mass spectrum (ESI, m/z): Calcd. for C11H13ClN2O2, 241.1 (M+H), found 241.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07427683B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-9562e868f3394d2dad6b7049c82ba3b0 |
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| 出典メモ | uspto-grants-2008_09 |
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