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. 80194-68-9, name is 3-Chloro-5-(trifluoromethyl)picolinic acid, the common compound, a new synthetic route is introduced below. Quality Control of 3-Chloro-5-(trifluoromethyl)picolinic acid
(1) Add 2 mmol) to a 25 ml three-necked flask3,5-Difluoro-5-(trifluoromethyl)picolinic acid8.0 mmol) pyridine and 5 ml acetonitrile, and the ice bath was cooled down to -5C. Then, 0.51 g (4.43 mmol) of methanesulfonyl chloride was slowly added dropwise to the system using a constant pressure dropping funnel. The mixture was stirred for 10 min after the addition was completed, and the mixture was once injected into the system. 3 mmol) 2-amino-3,5-difluorobenzoic acid was added, and after stirring for 10 min, 9 mmol) of pyridine was slowly added dropwise using a constant pressure dropping funnel. The dropping process should keep the temperature below 0C. Continue stirring after the addition was complete. 15min, then continue to slowly add 4.5mmol of methanesulfonyl chloride with a constant pressure dropping funnel, stir for 1h after dropping is completed, remove the ice salt bath, the reaction temperature slowly rises to room temperature, after 12h reaction, add water and dichloromethane extraction The organic layer was passed through a column (petroleum ether: ethyl acetate = 10: 1) to give the intermediate 6,8-difluoro-2-(3-chloro-5-(trifluoromethyl)pyridin-2-yl) -4H-benzo[d][1,3]oxazin-4-one.
The synthetic route of 80194-68-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Guizhou University; Wu Jian; Xu Fangzhou; Wang Yanyan; Yu Gang; Xue Wei; Shi Jun; (24 pag.)CN107759518; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem