Analyzing the synthesis route of 259808-67-8

259808-67-8, 259808-67-8 1-Boc-3,3-Dimethylpiperazine 22710387, apiperazines compound, is more and more widely used in various.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.259808-67-8,1-Boc-3,3-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

General procedure: In a 1 L round-bottom flask with a magnetic stir bar, compound 7 (46 g, 0.2014 mol, 1.0 eq.) was diluted in DIEA (41.64 mL, 0.2416 mol, 1.2 equivalents) and THF (700 mL). Solid N-Boc piperazine (39.38 g, 0.2114 mol, 1.05 eq.) was slowly added in portions. A mild exothermic reaction was observed. The reaction mixture was allowed to stir at room temperature for 2 hours then was quenched with saturated NaCl solution (100 mL), water (400 mL), and EtOAc (500 mL). The layers were separated and the aqueous layer was extracted with EtOAc (2 x 200 mL). The combined organic layers were dried (Na2SO4) and concentrated to give a gray solid. The crude solid was stirred in 2:1 TBME/hexanes (300/150 mL) overnight. The solids were filtered then washed with hexane (250 mL) to recover 52 g of impure product. The TBME/hexanes slurry was repeated to recover 46 g (59%) of compound 8. All remaining impure material was combined and purified via silica gel chromatography (4:1 hexane/EtOAc) to recover another 11.2 g (14%) of 8 for a total combined yield of 57.2 g (74%).

259808-67-8, 259808-67-8 1-Boc-3,3-Dimethylpiperazine 22710387, apiperazines compound, is more and more widely used in various.

Reference£º
Patent; ARAXES PHARMA LLC; DENG, Xiaohu; LI, Liansheng; LONG, Yun Oliver; LIU, Yuan; REN, Pingda; MANI, Neelakandha S.; ALLISON, Brett D.; SALES, Zachary S.; LIANG, Jimmy T.; (71 pag.)WO2017/100546; (2017); A1;,
Piperazine – Wikipedia
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