関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Acetylpiperazine | HCID 83795 | — |
| 反応物 | 4-Bromo-2-nitroanisole | HCID 118533 | — |
| 試薬 | Cesium carbonate | HCID 10796 | — |
| 触媒 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 触媒 | Palladium (II) acetate | HCID 4144353 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-[4-(4-Methoxy-3-nitro-phenyl)-piperazin-1-yl]ethanone | HCID 58235711 | 1.22% |
反応手順
4-bromo-1-methoxy-2-nitrobenzene (1.5 g, 6.46 mmol), 1-(piperazin-1-yl)ethanone (0.829 g, 6.46 mmol), CESIUM CARBONATE (4.21 g, 12.93 mmol), XANTPHOS (0.449 g, 0.78 mmol) and PdOAc2 (0.116 g, 0.52 mmol) were suspended in dioxane (20 ml) and sealed into a microwave tube. The reaction was heated to 120 °C for 90 minutes in the microwave reactor and cooled to RT. The reaction mixture was filtered through celite with ethyl acetate (50 mL). The filtrate was evaporated to dryness. The crude product was purified by flash silica chromatography in EtOAc. Pure fractions were evaporated to dryness to afford 1-(4-(4-methoxy-3-nitrophenyl)piperazin-1-yl)ethanone (0.022 g, 1.218 %) as a brown solid.
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-56a1dc90e93f4e37a4c4dceba5d45c4e |
|---|
| 出典メモ | 750 AstraZeneca ELN dataset |
|---|
