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1-(2-Methyl-5-nitro-phenyl)-piperidin-4-one → 3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(2-Methyl-5-nitro-phenyl)-piperidin-4-one | HCID 66656778 | — |
| 溶媒 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 生成物 | 3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one | HCID 67328898 | — |
反応手順
A solution of 1-(2-Methyl-5-nitro-phenyl)-piperidin-4-one [100 mg, 0.426 mmol] in N,N-Dimethylformamide dimethyl acetal (DMA.DMF) [1 ml] was heated to reflux for 12 hrs. After cooling to room temperature, reaction mixture was concentrated under vacuum. The dark brown crude product obtained was further purified by silica gel chromatography using 30-60% ethyl acetate/hexane as eluent to obtain pure desired product i.e., 3-Dimethylaminomethylene-1-(2-methyl-5-nitro-phenyl)-piperidin-4-one [4] as orange solid [Yield: 76.2 mg, 62.02%]
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08962637B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-b2b4d79805b2495988cffa207aa2cc19 |
| 出典メモ | uspto-grants-2015_02 |