Electric Literature of 176969-34-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 176969-34-9 name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid (0.211 g, 1.2 mmol) was added to the reaction flask in that order.Dichloromethane (6 ml), N,N-dimethylformamide (2 drops),Add oxalyl chloride (1 g, 8 mmol),The reaction solution was stirred at room temperature for 4 hours. The solvent is then removed by rotary evaporation to give 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid chloride.This was dissolved in dichloromethane (2 mL) for use.Then 4-fluoro-2-(2-pentyloxy)aniline (0.197 g, 1 mmol) was added to the reaction flask and triethylamine (0.13 mL) was added.Further, a solution of 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride was added dropwise to the reaction flask, and the mixture was stirred at room temperature for 16 hours.Then after monitoring the reaction by thin layer chromatography,Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate.The organic layer was washed with brine and dried over anhydrous sodium sulfate.Obtained 0.298 g of white solid.The yield was 83.94%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, and friends who are interested can also refer to it.
Reference:
Patent; Shanghai Taihe International Trade Co., Ltd.; Ma Wenjing; Lv Liang; Li Hongwei; Hou Shuang; Du Yonglei; Liu Jiyong; (31 pag.)CN108383791; (2018); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics