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. 16034-46-1 name is 1-Methyl-1H-pyrazole-5-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. 16034-46-1
Oxalyl chloride (0.088 g, 0.693 mmol) was added to a slurry of 1 -methyl- 1 H- pyrazole-5-carboxylic acid (0.066 g, 0.523 mmol) in dichloromethane (2 ml). One drop dimethylformamide was added and the reaction left to stir at room temperature for 2 hours. The reaction was concentrated in vacuo and azeotroped with dichloromethane. The residue was dissolved in THF (2 ml) and to this was added diisopropylethylamine (0.0956 g, 0.693 mmol) and 4- pyrrolidinopyridine (0.005 g, 0.035 mmol). The solution was cooled in an ice/acetone bath and 3-(2,3,5-trichlorophenyl)pyridine-2,6-diamine (Preparation 6, 0.100 g, 0.347 mmol) added portion-wise over 1 minute. The reaction was warmed to room temperature and stirred for 18 hours. The reaction was diluted with dichloromethane and washed with a saturated aqueous solution of NH4CI (10 ml), followed by a saturated aqueous solution of NaHCO3 (10 ml) and then water (10 ml) before drying over MgSO4 and concentrating in vacuo to afford a brown gum. The residue was purified by trituration with pentane to afford the title compound as a yellow oil. 1HNMR (ck-DMSO): 4.09 (s, 3H), 5.60 (br s, 2H), 7.22 (d, 1 H), 7.33 (d, 1 H), 7.38 (d, 1 H), 7.42 (d, 1 H), 7.50 (d, 1 H), 7.84 (d, 1 H), 10.30 (br s, 1 H)
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-1H-pyrazole-5-carboxylic acid, and friends who are interested can also refer to it.