5308-25-8,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5308-25-8,1-Ethylpiperazine,as a common compound, the synthetic route is as follows.
2-chloro-4 (4-fluorophenyl) -5,6,7,8,9,10-hexahydrocycloocta [b] pyridine (7.4 kg)BINAP (95 g), bis (dibenzylideneacetone) palladium(44 g), sodium tert-butoxide (3.7 kg),Toluene (37 L), ethyl piperazine (8.7 kg) was charged to the reactor.The temperature was raised to T = 75 to 80 C. and maintained at T = 80 to 85 C. for 3 hours.(Note: the reaction is exothermic, typically a complete conversion is achieved after 2 hours at 80 C). The mixture was cooled to 60-65 C.,Water (37 L) was added keeping the temperature at T = 60-65 C.The temperature was adjusted to T = 70-75 C. and the layers were separated. I removed the lower aqueous layer.The organic layer was washed with brine solution (36 L). Reduce the temperature below 25 C,The organic layer was filtered through an activated carbon cartridge.The organic layer was treated with water (22 L) and hydrochloric acid (4.5 L).The layers separated and the organic layer was removed. The aqueous layer (including product) was dissolved in toluene(37 L) and sodium hydroxide (5.2 L).The temperature was adjusted to T = 70-75 C. and the layers were separated. I removed the lower aqueous layer.The solvent was removed by vacuum distillation to a small amount. Acetone (22 L) was added,The mixture was heated to reflux. Dissolution occurred and the mixture was cooled to T = 0 to 5 C. The product was isolated by filtration and washed with cold acetone.The product in the wet state is dried under vacuum at T = 48-53 C. to give a purity99.92% A% HPLC (method 2) of blonanserin was obtained(7.8 kg, molar yield 85%). Blonanserin (7.6 kg) obtained in the above procedure was recrystallized from isopropanol (purpose: blank filtering of blonanserin) (6.7 kg; yield 88%; purity 99.94% A% HPLC (method 2)).
The synthetic route of 5308-25-8 has been constantly updated, and we look forward to future research findings.
Reference：
Patent; LUNDBECK PHARMACEUTICALS ITALY SA; HUBER, FLORIAN ANTON MARTIN; FAVERI, CARLA DE; (25 pag.)JP2018/43989; (2018); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics