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Iodoethane → 1-{2-[Ethyl-(4-pyridinyl)amino]benzoyl}piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium amide | HCID 24533 | — |
| 反応物 | 1-Piperidinyl(2-(4-pyridinylamino)phenyl)methanone | HCID 55754 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-{2-[Ethyl-(4-pyridinyl)amino]benzoyl}piperidine | HCID 13712468 | 100.8% |
反応手順
A solution of 22.4 g of 1-[2-(4-pyridinylamino)benzoyl]piperidine (Example 1b) in 45 ml of dimethylformamide was added dropwise to a suspension of sodium amide (from 4.8 g of 50% oil suspension, washed free of oil) in 115 ml of dimethylformamide. The mixture was stirred for one hour, and then 6.5 g of ethyl iodide was added dropwise. The reaction mixture was stirred for two hours, then filtered and concentrated in vacuo. The residue was partitioned between water and ether and the ether-soluble material recovered (15.2 g). The latter was recrystallized from ethyl acetate--pentane to give 13 g of 1-{2-[ethyl-(4-pyridinyl)amino]benzoyl}piperidine, m.p. 123°-124° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04610991 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-2648ece425c241b29fbe36b13df9c0cc |
| 出典メモ | uspto-grants-1986_09 |