These common heterocyclic compound, 113100-53-1, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Product Details of 113100-53-1
1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid (7.76 g, 40 mmol) represented by formula (III) was refluxed with thionyl chloride (47.6 g, 0.4 mol) for 4 hours, until the reaction system became a pale yellow transparent liquid, reaction was continued for 30 min, then the reaction was stopped, after cooling to room temperature, it is distilled under reduced pressure to give 1-methyl-3-trifluoromethyl-1H-pyrazole-4-acyl chloride, 1-methyl-3-trifluoromethyl-1H-pyrazole-4-acyl chloride (2 mmol) was added to 15 ml of dichloromethane, Phenylmethylamine (2.1 mmol) followed by triethylamine (0.3 g, 3 mmol) were slowly dropwise added at room temperature overnight; TLC (EpsilonAlpha: PE = 2:1(V) tracking, after the reaction was completed, it was extracted three times with a dichloromethane/water = 1:1 (V) system, and the organic layer was concentrated, extracted with toluene or 75% ethanol and subjected to column chromatography (EpsilonAlpha: PE = 2:1(V) to give N-benzyl-1-methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxamide represented by the formula(K1)
The synthetic route of 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Zhejiang University of Technology; Liu Xinghai; Jin Tao; Wang Han; Tan Chengxia; Weng Jianquan; Han Liang; (13 pag.)CN107935929; (2018); A;,
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