630125-91-6,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.630125-91-6,4-((4-Ethylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline,as a common compound, the synthetic route is as follows.
To a solution of 4-bromo-2- (difluoromethyl) aniline (100 mg 0.450 mmol) in THF (10 mL) was added triphosgene (46.8 mg 0.158 mmol) . The resulting mixture was stirred at 70 . After 30 min LCMS analysis showed the starting material was disappeared. The solvent was removed in vacuo to give 4-bromo-2- (difluoromethyl) -1-isocyanatobenzene (110mg 0.417 mmol 93yield) . To a solution of 4- ( (4-ethylpiperazin-1-yl) methyl) -3- (trifluoromethyl) aniline (153 mg 0.532 mmol) Et3N (0.124 mL 0.887 mmol) and DMAP (10.84 mg 0.089 mmol) in THF (10 mL) was added a solution of 4-bromo-2- (difluoromethyl) -1-isocyanatobenzene (110 mg 0.444 mmol) in THF (10 mL) . The resulting mixture was stirred at 70 . After LCMS analysis showed the starting material was disappeared. The solvent was removed in vacuo. The residue was purified by preparative TLC (DCM/MeOH 10/1) to yield a solid of 1- (4-bromo-2- (difluoromethyl) phenyl) -3- (4- ( (4-ethylpiperazin-1-yl) methyl) -3- (trifluoromethyl) phenyl) urea (130 mg 0.172 mmol 38.9yield) 1HNMR(400 MHz CD3OD) delta 7.86 (s 1H) 7.75 (d J 8.8 Hz 1H) 7.67-7.63 (m 4H) 7.03-6.76 (m 1H) 3.67 (s 2H) 3.20-3.18 (m 2H) 2.96 (m 8H) 1.30 (m 3H) ES-LCMS m/z 535.1 537.1 (M+H)
The synthetic route of 630125-91-6 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; GLAXOSMITHKLINE (CHINA) R & D COMPANY LIMITED; CHEUNG, Mui; DEMARTINO, Michael P.; EIDAM, Hilary Schenck; GUAN, Huiping Amy; QIN, Donghui; WU, Chengde; GONG, Zhen; YANG, Haiying; YU, Haiyu; ZHANG, Zhiliu; (391 pag.)WO2016/37578; (2016); A1;,
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