참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Acetylpiperazine | HCID 83795 | — |
| 반응물 | 4-Bromo-2-nitroanisole | HCID 118533 | — |
| 시약 | Cesium carbonate | HCID 10796 | — |
| 촉매 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 촉매 | Palladium (II) acetate | HCID 4144353 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 1-[4-(4-Methoxy-3-nitro-phenyl)-piperazin-1-yl]ethanone | HCID 58235711 | 1.38% |
반응 단계
4-bromo-1-methoxy-2-nitrobenzene (1.5 g, 6.46 mmol) was added in one portion to 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) in dioxane (20 ml) under nitrogen. The resulting mixture was stirred at 120 °C for 3 hours. The reaction mixture was filtered through celite and the fitrate evaporated to dryness. The crude product was purified by flash silica chromatography, elution gradient 0 to 10% MeOH in DCM. Pure fractions were evaporated to dryness to afford 1-(4-(4-methoxy-3-nitrophenyl)piperazin-1-yl)ethanone (0.025 g, 1.385 %) as a brown oil.
출처 및 근거
| 출처 데이터셋 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-05f07a62b42e4c23af01e32b4f5a3985 |
|---|
| 출처 메모 | 750 AstraZeneca ELN dataset |
|---|
