630125-91-6, 4-((4-Ethylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
To a solution of 2-fluoro-4- (4 4 5 5-tetramethyl-1 3 2-dioxaborolan-2-yl) aniline (500 mg 2.109 mmol) in THF (50 mL) was added triphosgene (219 mg 0.738 mmol) . The resulting miature was stirred at 70 . After 30min LCMS analysis showed the starting material was disappeared. The solvent was removed in vacuo to give 2- (3-fluoro-4-isocyanatophenyl) -4 4 5 5-tetramethyl-1 3 2-dioxaborolane (520 mg 1.977 mmol 94yield) . To a solution of 4- ( (4-ethylpiperazin-1-yl) methyl) -3- (trifluoromethyl) aniline (568 mg 1.977 mmol) Et3N (0.827 mL 5.93 mmol) and DMAP (24.15 mg 0.198 mmol) in THF (50 mL) was added a solution of 2- (3-fluoro-4-isocyanatophenyl) -4 4 5 5-tetramethyl-1 3 2-dioxaborolane (520 mg 1.977 mmol) at 70 . 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 dissolved in DCM (100 mL) and washed with H2O (30 mL) and brine (30 mL) . The organic layer was dried over Na2SO4 filtered and concentrated. The residue was purified by column chromatography (DCM/MeOH 20/1) to yiled 1- (4- ( (4-ethylpiperazin-1-yl) methyl) -3- (trifluoromethyl) phenyl) -3- (2-fluoro-4- (4 4 5 5-tetramethyl-1 3 2-dioxaborolan-2-yl) phenyl) urea (0.67 g 0.851 mmol 43.0yield) 1HNMR(400 MHz CD3OD) delta 8.17-8.14 (m 1H) 7.86 (s 1H) 7.69-7.67 (m 1H) 7.60 (d J 8.4 Hz 1H) 7.49 (d J 8.0 Hz 1H) 7.41 (d J 11.2 Hz 1H) 4.59 (s 2H) 3.60 (s 2H) 2.52-2.47 (m 8H) 1.33 (s 12H) 1.10 (t J 7.2 Hz 3H) ES-LCMS m/z m/z 551.2 (M+H), 630125-91-6
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;,
Piperazine – Wikipedia
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