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Ethyl chloroformate → Ethyl 4-(cyanomethyl)piperidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 1-Benzylpiperidine-4-acetonitrile | HCID 562499 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 4-(cyanomethyl)piperidine-1-carboxylate | HCID 18941011 | 81.4% |
反応手順
To a solution of 25 parts of 1-(phenylmethyl)-4-piperidineacetonitrile in 178 parts of tetrahydrofuran were added dropwise 37.97 parts of ethyl chloroformate at room temperature. The reaction mixture was stirred for 15 hours at room temperature and was then evaporated. The residue was taken up in 90 parts of ethyl acetate and the whole was washed successively with HCl 3N, NaHCO3 and NaCl (sat.). The solvent was evaporated and the residue was distilled (100°-110° C./6.7 Pa), yielding 18.7 parts (81.4%) of ethyl 4-(cyanomethyl)-1-piperidinecarboxylate (interm. 24).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05272150 |
| 出典データセット | uspto-grants-1993_12 |
| ORD ID | ord-6231955ae036458fa3203c65f9c0214e |
| 出典メモ | uspto-grants-1993_12 |