Reference of 956317-36-5, A common heterocyclic compound, 956317-36-5, name is 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid, molecular formula is C10H9N3O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
In the 50 L reaction flask A,10 kg of 5-methyl-2- (1,2,3-triazol-2-yl) benzoic acid,1.5 L dichloromethane,Ice bath to 0 ,Under nitrogen, 640 g of oxalyl chloride was added,100 g of DMF,The reaction was stirred at room temperature for 2 h.In another 100L reaction flask B,1.25 kg of compound 6 was added,1 kg of triethylamine,30 L of dichloromethane,Stir at room temperature for 2h and then cool the ice bath to 0 C,Dropping the mixture in the reaction flask A,Drop finished,Placed at 10 C,HPLC monitoring. After the reaction,The reaction solution was diluted with water,And then extracted with DCM,The DCM phase was dried over anhydrous sodium sulfate,And finally concentrated under reduced pressure at 45 C to obtain a crude product,The crude product was passed through a column of silica gel (60-120 mesh)The eluent was a 2% methanol / dichloromethane system,The compound 7 was concentrated in a brown oily liquid,Weight 1.98 kg, yield: 88%.
The synthetic route of 956317-36-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Chengdu Meiyugao Pharmaceutical Co., Ltd.; Chen Zhiyong; Wang Chunyan; Wang Cong; (26 pag.)CN106866632; (2017); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics