694499-26-8,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.694499-26-8,4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline,as a common compound, the synthetic route is as follows.
Unit Operation 3. 1: Drying Reaction Mixture AP25047, AP24592, and 2-methyl tetrahydrofuran (2-Me-THF) are charged to a reactor. The mixture is concentrated at reduced pressure to a target volume. Additional 2-methyl tetrahdyrofuran is added and the distillation repeated. Following another charge of 2-methyl tetrahydrofuran and a distillation cycle, the water content of the mixture is determined in IPC- 1 (KF). If the IPC-1 criterion is met, the process is continued to Unit Operation 3.2. Unit Operation 3.2: Reaction The suspension is maintained with stirring at a target temperature of 13 – 23C range while potassium fe -butoxide (KOfBu) is charged. After a period of not less than 3 hours, the reaction progress is determined by HPLC (IPC-2). If the IPC criterion is met, the process is continued to Unit Operation 3.3. Unit Operation 3.3: Quench and Extractions The reaction mixture is diluted with 2-methyltetrahydrofuran (2-Me-THF), and quenched by the addition of aqueous sodium chloride solution. The organic layer is separated and the aqueous layer is extracted twice with 2-methyl tetrahydrofuran. The combined organic layers are sequentially washed with aqueous sodium chloride and water. The organic layer is then aged at 15 – 30C. Unit Operation 3.4: Concentration / Solvent Exchange After aging (see Unit Operation 3.3), the mixture is passed through a cartridge filter and concentrated under vacuum to a target volume. 1 -Propanol is charged and allowed to stir at elevated temperature to furnish a solution, which is distilled under vacuum to a target volume and then cooled slowly to a temperature range of 20 – 30C. Unit Operation 3.5: Crystallization The product solution in 1 -propanol is aged with stirring at a temperature of 20 – 30C until the presence of solids is visually observed. Acetonitrile is charged to the suspension with stirring and the resulting suspension is aged for an additional 60 – 120 minutes at 20 – 30C with agitation prior to isolation in the next Unit Operation. Unit Operation 3.6: Isolation / Drying The slurry generated in Unit Operation 3.5 is isolated under vacuum in a filter/dryer. The solids are washed twice with a mixture of 1-propanol and acetonitrile. The solids are then dried under vacuum and monitored by IPC-3 (LOD, gravimetric). If the IPC criterion is met, the product is discharged as an off-white to yellow solid and packaged in double polyethylene bags for storage at ambient temperatures.
694499-26-8 4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline 46838908, apiperazines compound, is more and more widely used in various fields.
Reference：
Patent; ARIAD PHARMACEUTICALS, INC.; MURRAY, Christopher, K.; ROZAMUS, Leonard, W.; CHABER, John, J.; SHARMA, Pradeep; WO2014/93579; (2014); A2;,
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