関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Ethyl 1-(4-nitrophenyl)piperidine-4-carboxylate | HCID 2796870 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(4-Amino-phenyl)-piperidine-4-carboxylic acid ethyl ester | HCID 2764181 | 102.2% |
反応手順
To a solution of compound 18a (15.0 g, 51.2 mmol) in MeOH (100 mL) was added Fe (9.06 g, 162 mmol) and saturated NH4Cl solution (100 mL). The resulting solution was stirred at 80° C. for 5 h. After cooling to rt, the mixture was extracted with EtOAc (200 mL). The organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with EtOAc/petroleum ether (1:5 v/v) to obtain compound 18b as a black solid (13.0 g, 97% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C14H20N2O2: 249.2 (M+H). Found 249.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09249163B2 |
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| 出典データセット | uspto-grants-2016_02 |
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| ORD ID | ord-0b60d8e341604e9987b4ebe5f6c29319 |
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| 出典メモ | uspto-grants-2016_02 |
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