関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Acetylpiperazine | HCID 83795 | — |
| 反応物 | 2-Bromo-6-nitrotoluene | HCID 123537 | — |
| 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 | Toluene | HCID 1140 | — |
| 生成物 | 1-[4-(2-Methyl-3-nitrophenyl)piperazin-1-yl]ethanone | HCID 68592977 | 98.46% |
反応手順
1-bromo-2-methyl-3-nitrobenzene (500 mg, 2.31 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (201 mg, 0.35 mmol) and cesium carbonate (1131 mg, 3.47 mmol) and diacetoxypalladium (52.0 mg, 0.23 mmol) were dissolved in toluene (10 mL) and sealed into a microwave tube degazed and purged with argon. The reaction was heated to 100 °C, over a period of 12 hours. The reaction mixture was cooled down to room temperature, filtered and the residue was evaporated. The crude product was purified by flash chromatography on silica gel eluting with 0 to 10% methanol in dichloromethane. The solvent was evaporated to dryness to afford 1-(4-(2-methyl-3-nitrophenyl)piperazin-1-yl)ethanone (600 mg, 98 %) as a solid.
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
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| ORD ID | ord-57be3c43ca2f40d482cab5a1bd42b5d5 |
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| 出典メモ | 750 AstraZeneca ELN dataset |
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