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Cesium carbonate → 1-{[3-Acetyl-6-(2-chlorophenyl)-5-(4-chlorophenyl)pyridin-2-yl]oxy}-3,3-dimethylbutan-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Bromopinacolone | HCID 21642 | — |
| 反応物 | 3-Acetyl-6-(2-chlorophenyl)-5-(4-chlorophenyl)pyridin-2(1H)-one | HCID 67019915 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-{[3-Acetyl-6-(2-chlorophenyl)-5-(4-chlorophenyl)pyridin-2-yl]oxy}-3,3-dimethylbutan-2-one | HCID 21984817 | — |
反応手順
To a 25 mL rb flask equipped with a magnetic stir bar was added 0.309 g(0.86 mmol) of the product of Step A, 0.422 g (1.29 mmol) of cesium carbonate, 3 mL DMF and finally 145 μL of 1-bromopinacolone was added. The reaction mixture was stirred at room temperature for 1.5 h then partitioned between EtOAc and water. The organic layer was separated, washed with 10% aq. NaHSO4, water, brine, dried (MgSO4), filtered and evaporated. The residue was purified on s silica gel flash chromatography column eluted with 0–10% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091216B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-ea6785e61a9d489682d374698133b827 |
| 出典メモ | uspto-grants-2006_08 |