1-Acetylpiperazine → 1-[4-(4-Methoxy-3-nitro-phenyl)-piperazin-1-yl]ethanone

HRID 192

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HRID 192 반응식
CC(=O)N1CCNCC1.COc1ccc(Br)cc1[N+](=O)[O-]>C1COCCO1.CC(=O)O.CC(=O)O.CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21.O=C([O-])[O-].[Cs+].[Cs+].[Pd]>COc1ccc(N2CCN(C(C)=O)CC2)cc1[N+](=O)[O-]

참가 물질

7

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온도
120 °C

실험 절차

diacetoxypalladium (2.322 g, 10.34 mmol) was added to a stirred suspension of 4-bromo-1-methoxy-2-nitrobenzene (30 g, 129.29 mmol), 1-(piperazin-1-yl)ethanone (16.57 g, 129.29 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (8.98 g, 15.52 mmol) and cesium carbonate (84 g, 258.59 mmol) dissolved in dioxane (300 mL) , degased and under argon. The resulting suspension was stirred at 120 °C for 2 hours.At 25°C, the mixture was filtered and adsorbed on silica gel .The crude product was purified by flash chromatography on silica gel eluting with 1 to 5% methanol in ethyle acetate. The solvent was evaporated to dryness to afford 1-(4-(4-methoxy-3-nitrophenyl)piperazin-1-yl)ethanone (31.0 g, 86 %) as a orange solid.

출처 및 근거

ORD 기록
ord-77e8bb12d76a4a1d94f2c62d1d96fda1
출처 데이터셋
750 AstraZeneca ELN dataset
원본 링크
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