Reference of 63489-58-7, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.63489-58-7, name is 2,6-Difluoropyridin-4-amine, molecular formula is C5H4F2N2, molecular weight is 130.0955, as common compound, the synthetic route is as follows.
Nitrogen protection conditions, In a dry autoclave, 300 ml of anhydrous sulfolane was added successively, 2,6-difluoro-4-amino pyridine (29.2g, 200mmol), Compound N (N-(5-tert-butyl-1,3,4-thiadiazol-2-yl)-4-methyl-1,2,3-thiadiazole-5-formamide) (56.7 g of , 200mmol), The freshly distilled thionyl chloride (59.5 g, 500 mmol) and DCC (dicyclohexylcarbodiimide) (41.3 g, 200 mmol) were heated under reflux for 4.5 hours, The reaction was changed from reflux to distillation, Distillation of the low boiling point components in the reactor (the main component is unreacted thionyl chloride) Heating to 100 C reaction 2 to 4 hours, Liquid chromatography control detection, Until the reaction of the starting material (compound N) is complete, Stop the reaction. Slightly cold, The reaction solution was poured into a large amount of crushed ice, The pH was adjusted to 7 with 1 M aqueous sodium hydroxide solution, Filter, The product was recrystallized from an aqueous ethanol solution, to give N-(5-tert-butyl-1,3,4-thiadiazol-2-yl)-N’-(2,6-difluoropyridin-4-yl)-4-methyl-1,2,3-thiadiazole-5-carboxamidine (M-10), White solid 69.0 g, Liquid normalized content of 99.0% Yield 87.3%.
The chemical industry reduces the impact on the environment during synthesis 63489-58-7, I believe this compound will play a more active role in future production and life.
Reference:
Patent; Xihua University; Liu, Ping; Yang, Weiqing; Ma, Menglin; Zhang, Yuanyuan; Zhang, Yan; (11 pag.)CN104530040; (2017); B;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem