With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5464-12-0,1-(2-Hydroxyethyl)-4-methylpiperazine,as a common compound, the synthetic route is as follows.,5464-12-0
Example 412-(4-Methylpiperazin-1-yl)ethyl 4-(4-fluorophenyl)piperazine-1-carboxylate 2-(4-Methyl-piperazin-1-yl)-ethanol (1.44 g, 10 mmol) was dissolved in anhydrous THF (50 mL) and the reaction mixture was cooled to 0¡ã C. NaH (60percent dispersion in oil; 0.40 g, 10 mmol) was added and stirred for 10 minutes and then 4-(4-fluorophenyl)-piperazine-1-carboxylic acid 4-nitrophenyl ester (3.45 g, 10 mmol) was added. The reaction mixture was stirred at room temperature overnight. The reaction mixture was cautiously quenched by the dropwise addition of a water (1 mL)/THF (10 mL) mixture. The THF was removed in vacuo and the residue was suspended between sat aq Na2CO3 solution (50 mL) and EtOAc (200 mL). The organic layer was washed with sat aq Na2CO3 solution (5.x.50 mL), dried (MgSO4) and the solvent removed in vacuo.The residue was initially purified by reverse phase column chromatography (LiChroprep RP-18, 40-63 mum, 460.x.26 mm (10g), 30 mL/min, gradient 0percent to 60percent (over 60 min) MeOH in water). Further purification by reverse phase column chromatography in two batches (LiChroprep RP-18, 40-63 mum, 460.x.26 mm (100 g),30 mL/min, gradient 0percent to 20percent (over 70 min) to 100percent (over 5 min) MeOH in water with 1percent formic acid) gave pure 2-(4-methylpiperazin-1-yl)ethyl 4-(4-fluorophenyl)piperazine-1-carboxylate formate. The formic acid was removed using K2CO3 in DCM and then dried in a vacuum oven overnight to give 2-(4-methylpiperazin-1-yl)ethyl 4-(4-fluorophenyl)piperazine-1-carboxylate (0.60 g, 17percent) as a colourless gum.Analytical HPLC: purity 99.5percent (System A, RT=3.70 min); Analytical LCMS: purity 100percent (System A, RT=4.08 min), ES+: 351.1 [MH]+; HRMS calcd for C18H27FN4O2: 350.2118, found 350.2133.
As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.
Reference£º
Patent; Biovitrum AB; US2009/281087; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics