関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 5-Chloro-2-nitrobenzoic acid | HCID 17286 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 2-Nitro-5-(piperidin-1-yl)benzoic acid | HCID 14459331 | — |
反応手順
A mixture of 5-chloro-2-nitrobenzoic acid (13.7 g), piperidine (27 ml) and DMA (100 ml) was stirred and heated to 120° C. for 18 hours. The mixture was evaporated. The residue was dissolved in water and the solution was basified to pH10 by the addition of 2N aqueous sodium hydroxide solution. The solution was extracted with ethyl acetate. The aqueous layer was acidified to pH2 by the addition of concentrated hydrochloric acid and extracted with ethyl acetate. The organic layer was dried (MgSO4) and evaporated to give 2-nitro-5-piperidinobenzoic acid (16.25 g), m.p.130°-140° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05616582 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-e548eecaff784fc8846e4a93534b5491 |
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| 出典メモ | uspto-grants-1997_04 |
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