Synthetic Route of 128694-63-3, A common heterocyclic compound, 128694-63-3, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid, molecular formula is C6H5F3N2O2, 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.
EXAMPLE 2 N-[5-(2-chloro-6-fluorophenyl)-1H-pyrazol-3-yl]-1-methyl-3-(trifluoromethyl)-1H-pyrazole-5-carboxamide [0113] Compound of Preparation 11 (100 mg, 0.19 mmol) and 1-methyl-3-(trifluoromethyl)-1 H-pyrazole-5-carboxylic acid (91 mg, 0.47 mmol) were dissolved in 1.5 mL DMF. N-(3-Dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride 98% (144 mg, 0.75 mmol) and 1-Hydroxybenzotriazole hydrate (102 mg, 0.75 mmol) were added and the mixture was stirred at room temperature overnight. Ethyl acetate was added and the organic phase was washed with water two times, NaOH 1 N two times, dried over MgSO4 and evaporated under reduced pressure and the residue was purified using the Isolera purification (ethyl acetate – hexane gradient, 0:100 rising to 100:0) to give 35 mg (0.09 mmol, 19%) of the title compound as a white solid. LRMS (m/z): 388 (M+1)+. 1 H NMR (300 MHz, DMSO-d6) d ppm 4.19 (3 H, s), 6.86 (1 H, s), 7.31 – 7.61 (3 H, m), 7.65 (1 H, s), 11.24 (1 H, br. s), 12.97 (1 H, br. s)
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.