With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.169447-70-5,(S)-tert-Butyl 2-methylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.
Compound bromo-2-fluoro-3-nitrobenzene 64a (3.1 g, 14.0 mmol), 1-tert-butoxycarbonyl (2S)-2-methylpiperazine(4.2 g, 21.0 mmol) and dioxane (50 mL) were mixed, and tris(bisbenzylideneacetone)palladium (0.6 g,0.7 mmol), 4,5-bisdiphenylphosphino-9,9-dimethyloxaxan (0.8 g, 1.4 mmol) and cesium carbonate (9.1 g, 28 mmol),The reaction was carried out under an argon atmosphere at 110 C for 16 hours. Cool to room temperature, extract with dichloromethane (100 mL¡Á3), and use organic phaseWash with saline solution (100 mL). Dry the organic phase with anhydrous sodium sulfate, remove the desiccant by filtration, and pass the residue through a flash column.Chromatography purification (petroleum ether / ethyl acetate = 5:1) afforded the desired product 1-t-butoxy acyl (2S)-4-(2-fluoro-3-nitrobenzene2-methylpiperazine 64b (2.6 g, 7.7 mmol, red oily liquid), yield: 55%.
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Patent; Nanjing Tianyinjianhua Pharmaceutical Technology Co., Ltd.; Kong Xianglong; Zhou Chao; Zheng Zhixiang; (105 pag.)CN109020957; (2018); A;,
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