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N,N'-Dimethylethylenediamine → 3-{4-[4-(3,5-Dimethylpyridin-2-yl)piperazine-1-carbonyl]-3,5-difluorophenyl}oxazolidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Oxazolidinone | HCID 73949 | — |
| 反応物 | (4-Bromo-2,6-difluorophenyl)[4-(3,5-dimethylpyridin-2-yl)piperazin-1-yl]methanone | HCID 58484761 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-{4-[4-(3,5-Dimethylpyridin-2-yl)piperazine-1-carbonyl]-3,5-difluorophenyl}oxazolidin-2-one | HCID 67380885 | 55.1% |
反応手順
To a mixture of (4-bromo-2,6-difluorophenyl)[4-(3,5-dimethylpyridin-2-yl)piperazin-1-yl]methanone (410 mg) described in Preparation Example 60, oxazolidin-2-one (87 mg), potassium carbonate (277 mg) and copper (I) iodide (95.8 mg) were added toluene (1 mL) and N,N′-dimethylethylenediamine (101 μL), and the mixture was refluxed for 8 hr. Water was added to the reaction mixture, the mixture was extracted with chloroform, and the solvent was evaporated. The residue was purified by column chromatography (chloroform:methanol) to give the title compound (229.3 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08354401B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-4c32dbeac0ff4fe1a2c363e6455070e1 |
| 出典メモ | uspto-grants-2013_01 |