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Hydrochloric Acid → 1-Benzyloxycarbonyl-4-[methoxycarbonyl(ethylamino)]-piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Benzyl 4-(methoxycarbonylamino)piperidine-1-carboxylate | HCID 18677680 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Benzyloxycarbonyl-4-[methoxycarbonyl(ethylamino)]-piperidine | HCID 18677725 | 97% |
反応手順
To 82 mg (0.28 mmol) of 1-benzyloxycarbonyl-4-(methoxycarbonylamino)piperidine from Step A and 0.045 mL (0.56 mmol) of ethyl iodide in 4 mL of DMF under nitrogen was added 22 mg (0.56 mmol) of 60% sodium hydride in mineral oil. The reaction was stirred at rt for 1 h and was then poured into water containing 1 mL of 2 N hydrochloric acid and extracted twice with ether. The organic layers were each washed with a portion of brine, dried over sodium sulfate, combined and concentrated. The residue was purified by FC eluting with 50% ethyl acetate in hexanes to afford 87 mg of title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06472410B1 |
| 出典データセット | uspto-grants-2002_10 |
| ORD ID | ord-db214a4b864645a8968948348e8bc713 |
| 出典メモ | uspto-grants-2002_10 |