Synthetic Route of 176969-34-9, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows.
a synthesis reaction experimental device is connected in a circulating cooling reaction pump at 0 C, and nitrogen gas is introduced in the early stage.To remove the air from the reaction flask, keep nitrogen in, and add 1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid to the round bottom flask after about 5 minutes.(LM-1-a) 0.528 g (3 mmol), 20 mL of re-distilled dichloromethane,Re-steaming DMF 0.482 mL (6 mmol),The reaction liquid was stirred and 0.316 mL (3.6 mmol) of oxalyl chloride was slowly added dropwise thereto using a dropping funnel. After 1.5h-2.5h reactionThe reaction was closed, and the insoluble material was removed by suction under reduced pressure. The filtrate was slowly added dropwise to a solution of 0.856 g (2.4 mmol) of N-(2-fluorophenyl)-2-aminocyclohexanesulfonamide and 0.6 mL with a dropping funnel. 4.32mmol) triethylamine in a mixed solution of dichloromethane, continue to be lowAfter stirring for 15 min, the reaction was changed to room temperature for about 2 h, and the reaction was monitored by TLC [V (petroleum ether): V (ethyl acetate) = 2:1].During the reaction, the reaction of the raw materials is judged according to the condition of the plate. After the reaction is completed, the reaction is stopped. AdditionalAppropriate amount of methylene chloride, the reaction solution was washed with HCl, washed with NaHCO3, washed with water, dried over anhydrous sodium sulfate, and allowed to stand for more than 8h.The crude product is purified by column chromatography, and the product is recrystallized from dichloromethane or acetone to give a white powdery solid.Pure productN-(2-Trifluoromethyl-4-chlorophenyl)-2-[1-methyl-3-difluoromethyl-4-pyrazolecarboxamido]cyclohexanesulfonamide.
The chemical industry reduces the impact on the environment during synthesis 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid. I believe this compound will play a more active role in future production and life.