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4-Methylmorpholine → 1-(5-Methyl-2-(pyridin-4-yl)benzoyl)piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride | HCID 2734059 | — |
| 反応物 | 4-Piperidone hydrochloride | HCID 3084851 | — |
| 反応物 | 5-Methyl-2-(pyridin-4-yl)benzoic acid hydrochloride | HCID 86680842 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(5-Methyl-2-(pyridin-4-yl)benzoyl)piperidin-4-one | HCID 86680848 | 31% |
反応手順
A suspension of 5-methyl-2-(pyridin-4-yl)benzoic acid hydrochloride (2.0 g), piperidin-4-one hydrochloride (1.2 g), DMTMM (3.3 g) and N-methylmorpholine (2.6 mL) in DMF (30 mL) was stirred at room temperature for 5 hr, and then overnight at 100° C. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (0.73 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08648079B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-e5f3a5eb1548437391af722717e65e5d |
| 出典メモ | uspto-grants-2014_02 |