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Potassium Carbonate → N,N-bis(3-methylbutyl)-4-nitro-3-[(3-piperidin-1-ylpropyl)amino]benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Piperidine-1-propylamine | HCID 19049 | — |
| 反応物 | 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide | HCID 68447111 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N,N-bis(3-methylbutyl)-4-nitro-3-[(3-piperidin-1-ylpropyl)amino]benzamide | HCID 68446148 | 78% |
反応手順
A mixture of 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide (430 mg, 1 eq, prepared according to Example A1), 3-piperidino-propylamine (212 mg, 1.1 eq) and potassium carbonate (365 mg, 2 eq) in acetonitrile (10 ml) is heated under reflux for 3 hours then concentrated under reduced pressure at 40° C. The residue is taken up in dichloromethane (50 ml) and water (20 ml). After decantation and extractions, the combined organic phases are washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40° C. Purification of the residue by flash chromatography on silica gel (eluent: ethyl acetate 100%) produces the expected compound in the form of a yellow oil (460 mg; 78% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07501524B2 |
| 出典データセット | uspto-grants-2009_03 |
| ORD ID | ord-4c860cc4d2c9450a8016f21b48a21c1b |
| 出典メモ | uspto-grants-2009_03 |