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HRID 71作成日:2026年10月23日

1-Acetylpiperazine → 1-[4-(2-Methyl-3-nitrophenyl)piperazin-1-yl]ethanone

https://huagongshe.com/ja/reaction/71

反応式

関与物質

役割名称HCID仕込み量
反応物1-AcetylpiperazineHCID 83795—
反応物2-Bromo-6-nitrotolueneHCID 123537—
試薬Cesium carbonateHCID 10796—
触媒1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 636044—
触媒Palladium (II) acetateHCID 4144353—
溶媒TolueneHCID 1140—
生成物1-[4-(2-Methyl-3-nitrophenyl)piperazin-1-yl]ethanoneHCID 6859297798.46%

反応条件

温度100 °C

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
ORD IDord-57be3c43ca2f40d482cab5a1bd42b5d5
出典メモ750 AstraZeneca ELN dataset