Reference of 60166-43-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 60166-43-0, name is 1,4-Dimethyl-1H-1,2,3-triazole belongs to Triazoles compound, it is a common compound, a new synthetic route is introduced below.
To a 20 mL scintillation vial was added (S)-3-bromo-7-chloro-5- (phenyl(tetrahydro-2H-pyran-4-yl)methyl)-5H-pyrrolo[2,3-b:4,5-b’]dipyridine (0.223 mmol, 102 mg) l,4-dimethyl-lH-l,2,3-triazole (0.223 mmol, 21.7 mg), Me4NOAc (0.223 mmol, 29.7 mg) and PdCh(PPh3)2 (0.016 mmol, 11.0 mg) followed by the addition of 4 mL NMP. The air was replaced with argon. The sealed reaction vial was heated to 100 C with stirring overnight. It was cooled to room temperature and diluted with EtOAc and washed twice with brine. The organic layer was dried over MgS04, and concentrated. It was subjected to purification on the IS CO, 24 g silica gel column, eluting with 50- 100% EtOAc/hexanes, then 0-10% MeOH/EtOAc to obtain the title compound, 139 mg in 60 % purity. A second ISCO was run using a 24 g silica gel column eluting with 0- 100% (10% 2M NH3 in EtOAc)/DCM to obtain the title compound (thick oil), 58 mg. LC/MS (M+H) = 473.2 [Column: Waters Aquity BEH CI 8 2.1 X 50 mm 1.7u; Mobile Phase A: water with 0.05% TFA; Mobile Phase B: ACN with 0.05% TFA; Temperature: 40 C; Gradient: 2-98% B over 1.5 min; Flow: 0.8 mL/min].
The synthetic route of 1,4-Dimethyl-1H-1,2,3-triazole has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; NORRIS, Derek J.; VACCARO, Wayne; DEBENEDETTO, Mikkel V.; DEGNAN, Andrew P.; DELUCCA, George V.; DESKUS, Jeffrey A.; HAN, Wen-Ching; KUMI, Godwin Kwame; SCHMITZ, William D.; STARRETT, John E., JR.; HILL, Matthew D.; HUANG, Hong; (563 pag.)WO2016/183118; (2016); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics