With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.6531-38-0,2,2′-(Piperazine-1,4-diyl)diethanamine,as a common compound, the synthetic route is as follows.
To a 25ml RBF containing a magnetic stir bar was added the imidazolide of Bumetanide (0.207g , 0.99mmol) and dissolved in ImI DCM. To the above solution was added the amine (0.172g, 0.999mmol) and let stir overnight at it under argon. TLC in 10% MeOH in EtOAc indicated a very polar spot. Extracted the reaction mixture into EtOAc, washed with water (2x20ml) and then with brine (2x20ml). The organic layer was dried under MgSO4 and filtered. Concentrated the organic layerunder vacuum. Redissolved the crude product in the minimum amount of DCM and reprecipitated from hexanes. Filtered the above precipitate to obtain yellowish white solid. 1HNMR in DMSO-d6+2 drops of MeOD.1HNMR (300MHz, DMSO-d6+2 drops of MeOD) Q.80ppm (t, J=IOHz, 3H),1.1 lppm (m, 2H), 1.37rhopm (m,2H), 2.50ppm (m, 8H), 3.05ppm (t, J= 6.6Hz, 2H), 3.35ppm (t, J=.6Hz, 2H), 4.1ppm (s, br, 4H), 4.95ppm (t, br, IH), 6.85ppm (d, J=7.8Hz, 2H), 7.00ppm (t, 7.2Hz, IH), 7.26ppm (dd, J=7.8Hz, 2H), 7.6ppm (s, IH) 13CNMR (75MHz, DMSO-d6) 19.23, 24.93, 35.89, 47.50, 58.45, 62.50,107.50, 1 19.0, 121.16, 128.0, 134.66, 137.50, 144.0, 143.00, 147.80, 162.20, 171.0 FABMS 519 (M+H)+ calcd m/z for C25H39N6O4S+ 519.28 ; found 519.27, 6531-38-0
6531-38-0 2,2′-(Piperazine-1,4-diyl)diethanamine 81020, apiperazines compound, is more and more widely used in various fields.
Reference：
Patent; FLYNN, Gary, A.; YOOL, Andrea, J.; MIGLIATI, Elton, Rodrigues; RITTER, Leslie, S.; WO2008/52190; (2008); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics