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1H-Pyrazole-4-carboxamide,1,3-dimethyl-(9CI) synthesis

4synthesis methods
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Yield:124845-21-2 1.39 g

Reaction Conditions:

Stage #1: 1,3-dimethyl-1H-pyrazole-4-carboxylic acid chloridewith ammonium hydroxide;potassium carbonate in tetrahydrofuran at 0;
Stage #2: in tetrahydrofuran at 20; for 2 h;Cooling with ice;

Steps:



In a 500 mL single-necked flask, 34 g of 25% aqueous ammonia and 15.2 g of K2CO3 were added,Further diluted with 100 mL of THF,After stirring, the mixture was cooled to 0 ° C,A mixture of the above-mentioned pale yellow solid was dissolved in 100 mL of THF under ice bath,There is a white solid,After dripping at room temperature for 2 h,TLC detection reaction completely, vacuum distillation to remove THF,Produce a large amount of solid, filter, washed, dried,A white solid.A solution of 1.39 g (10 mmol) of 1,3-dimethyl-1H-pyrazole-4-carboxamide (5)

References:

CN107033084,2017,A Location in patent:Paragraph 0029