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Methanol → Ethyl 4-[(2,6-dichlorophenyl)amino]-1-piperidinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Ethyl 4-[(2,6-dichlorophenyl)imino]-1-piperidinecarboxylate | HCID 23339072 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Ethyl 4-[(2,6-dichlorophenyl)amino]-1-piperidinecarboxylate | HCID 23338997 | — |
反応手順
To a stirred and refluxing mixture of 250 parts of ethyl 4-[(2,6-dichlorophenyl)imino]-1-piperidinecarboxylate in 160 parts of methanol and 160 parts of 2-propanol are added portionwise 30 parts of sodium borohydride. Upon completion, stirring at reflux temperature is continued for one hour. The warm reaction mixture is poured onto water and the product is extracted with methylbenzene. The extract is dried and evaporated. The residue is crystallized from a mixture of 160 parts of 2,2'-oxybispropane and 160 parts of petroleumether, yielding 96 parts of ethyl 4-[(2,6-dichlorophenyl)amino]-1-piperidinecarboxylate; mp. 107.2°-116.6° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04151286 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-0fc4a7895f4a4ca7afdf6601906011b4 |
| 出典メモ | uspto-grants-1979_04 |