Adding a certain compound to certain chemical reactions, such as: 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, belongs to pyrazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 176969-34-9, SDS of cas: 176969-34-9
N dichloromethane 1ml solution of 3-difluoromethyl-1-methyl -1H- pyrazole-4-carboxylic acid 176mg, added N- dimethylformamide 10mg and oxalyl chloride 381mg, I was stirred at room temperature for 1 hour.After completion of the reaction, distilling off the solvent under reduced pressure, the residue was dissolved in dichloromethane 2ml, 2- amino-1- (3,5-dichloropyridine prepared with stirring under ice-cooling, at step 5 Synthesis Example 2 2-yl) ethanone -O- dichloromethane 2ml solution of ethyl oxime 190mg, then dropped the pyridine 91mg, was continued for a further 2 hours stirring at room temperature after completion of the dropping.After completion of the reaction, and extracted with added water 10ml reaction mixture chloroform (20mlx1), after the organic layer washed with water (10mlx1), and dehydrated and dried in this order brine then anhydrous sodium sulfate, and distilling off the solvent under reduced pressure It was.The residue was ethyl acetate – hexane (1: 4 to 1: 1 gradient) was purified by silica gel column chromatography eluting with, to give a pale yellow resinous substance 165.3mg.The thing is dissolved in acetic acid 5ml, After stirring for 2 hours at 70 , distilling off the solvent under reduced pressure, the residue partitioned between ethyl acetate – hexane (1: 4 to 1: 1 gradient) and eluting with It was purified by silica gel column chromatography, and the desired compound 130.6mg obtained as a colorless resin-like substance (E / Z = 1/1).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; NISSAN CHEMICAL INDUSTRIES LIMITED; Iwasa, Motoyoshi; Tomizawa, Mitsutaka; Tsuji, Keisuke; Nakamura, Toshiyuki; Mita, Takeshi; Kuwahara, Hidehito; asahi, Miho; Imanaka, Hotaka; (342 pag.)JP2016/11286; (2016); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics