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With ammonium hydroxide; hydrogen In methanol at 40℃; for 8 h; Autoclave
To a solution of A6.2 (228 g, crude) and 145 mL NH4OH in 1.0 L MeOH was added 30 g Raney Ni. The mixture was stirred in an autoclave at 40 oC under hydrogen atmosphere (25 atm) for 8 h. After filtration, the filtrate was concentrated under reduced pressure to get a pale yellow oil, which was purified by reduced pressure distillation to give the title compound (60 g, 54 percent) as a colorless oil.1H NMR (500 MHz, DMSO-d6) δ ppm 1.58 (s, 2H), 3.67 (s, 1H), 6.75 (t, 1H), 6.82 (d, 1H), 7.22 (dd, 1H). LC- MS: [MH]+ = 156.1
60 g
With hydrogen In methanol at 40℃; for 8 h; Autoclave
To a solution of A3.2 (228 g, crude) and 145 mL NH4OH in1 .0 L MeOH was added 30 g Raney Ni. The mixture was stirred in an autoclave at 40 °Cunder hydrogen atmosphere (25 atm) for 8 h. After filtration, the filtrate was concentrated under reduced pressure to get a pale yellow oil, which was purified by reduced pressure distillation to give the title compound (60 g, 54 percent) as a colorless oil. 1H NMR (500 MHz, DMSO-d6) O ppm 1.58 (5, 2H), 3.67 (5, 1H), 6.75 (t, 1H), 6.82 (d, 1H), 7.22 (dd, 1H). LC10 MS: [MH] 156.1.
With ammonium hydroxide; hydrogen; In methanol; at 40.0℃; under 19001.3 Torr; for 8.0h;Autoclave;
To a solution of A6.2 (228 g, crude) and 145 mL NH4OH in 1.0 L MeOH was added 30 g Raney Ni. The mixture was stirred in an autoclave at 40 oC under hydrogen atmosphere (25 atm) for 8 h. After filtration, the filtrate was concentrated under reduced pressure to get a pale yellow oil, which was purified by reduced pressure distillation to give the title compound (60 g, 54 %) as a colorless oil.1H NMR (500 MHz, DMSO-d6) delta ppm 1.58 (s, 2H), 3.67 (s, 1H), 6.75 (t, 1H), 6.82 (d, 1H), 7.22 (dd, 1H). LC- MS: [MH]+ = 156.1
60 g
With hydrogen; In methanol; at 40.0℃; under 19001.3 Torr; for 8.0h;Autoclave;
To a solution of A3.2 (228 g, crude) and 145 mL NH4OH in1 .0 L MeOH was added 30 g Raney Ni. The mixture was stirred in an autoclave at 40 Cunder hydrogen atmosphere (25 atm) for 8 h. After filtration, the filtrate was concentrated under reduced pressure to get a pale yellow oil, which was purified by reduced pressure distillation to give the title compound (60 g, 54 %) as a colorless oil. 1H NMR (500 MHz, DMSO-d6) O ppm 1.58 (5, 2H), 3.67 (5, 1H), 6.75 (t, 1H), 6.82 (d, 1H), 7.22 (dd, 1H). LC10 MS: [MH] 156.1.
8-bromo-5-chloro-[1,2,4]triazolo[4,3-a]pyridine[ No CAS ]
8-bromo-N-(2-fluoro-6-methoxybenzyl)-[1,2,4]triazolo[4,3-a]pyridin-5-amine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
30%
In ethanol; at 85.0℃; for 8.0h;
To a solution of 3a (1 g, 4.33 mmol) in EtOH (0.5 mL) was added (2-fluoro-6- methoxyphenyl)methanamine (1.5 g, 9.68 mmol) and the mixture was stirred at 85 oC for 8 h.5 mL of EtOAc was added and filtered to give a white solid, which was purified by flash chromatography to afford the title compound (0.45 g , 30%).1H-NMR (400 MHz, DMSO-d6) delta ppm 3.88 (s, 3H), 4.45 (s, 2H), 5.98 (d, 1H), 6.89 (t, 1H), 6.96 (d, 1H), 7.36 - 7.45 (m, 1H), 7.60 (d, 1H), 9.55 (s, 1H). LC-MS: [MH]+ = 351.
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