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 43 2-(4-Methylpiperazin-1-yl)ethyl 4-(4-chlorobenzyl)piperazine-1-carboxylate 2-(4-Methyl-piperazin-1-yl)-ethanol (0.86 g, 6 mmol) and NMM (0.58 mL, 6 mmol) were dissolved in DCM (8 mL) and the reaction mixture was cooled to 0¡ã C. 4-Nitrophenyl chloroformate (1.29 g, 6 mmol) was added and stirred for 1 h. To the reaction mixture was added a solution of 1-(4-chloro-benzyl)-piperazine (1.05 g, 5 mmol) and DIPEA (6.0 mL, excess) in DMF (20 mL). The reaction mixture was stirred at room temperature overnight and then concentrated in vacuo. The residue was dissolved in EtOAc (150 mL), washed with sat aq Na2CO3 solution (6*100 mL), dried (MgSO4) and dried in vacuo. The residue was initially purified by column chromatography (normal phase, 20 g, Strata SI-1, silica gigatube, 20 mL/min, gradient 0percent to 15percent MeOH in DCM) and then further purified by reverse phase column chromatography (LiChroprep RP-18, 40-63 mum, 460*26 mm (100 g), 30 mL/min, gradient 0percent to 30percent (over 40 min) MeOH in water with 1percent formic acid). The residue was stirred for 2 h in DCM (10 mL) with K2CO3 (~0.20 g), filtered and then dried in a vacuum oven overnight to give 2-(4-methylpiperazin-1-yl)ethyl 4-(4-chlorobenzyl)piperazine-1-carboxylate (0.51 g, 28percent) as a pale yellow oil. Analytical HPLC: purity 99.7percent (System A, RT=3.39 min); Analytical LCMS: purity 100percent (System A, RT=3.83 min), ES+: 381.5 [MH]; HRMS calcd for C19H29ClN4O2: 380.1979, found 380.1996.
The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Biovitrum AB; US2009/281087; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics