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2,5-Dimethyl-1,3-dinitrobenzene synthesis

6synthesis methods
-

Yield:609-92-7 54.67%

Reaction Conditions:

with sulfuric acid;nitric acid in water at 20 - 80; for 1 h;Temperature;

Steps:

1-8

In a 250 mL four-necked flask equipped with a thermometer, 18.96 mL of HNO3 was put, and 44.48 mL of concentrated sulfuric acid was poured in an ice water bath with stirring. After the concentrated nitric acid and concentrated sulfuric acid were mixed evenly, 15 mL of para-xylene was dropped into it with a constant-pressure dropping funnel, the dropping temperature was controlled to be 20 to 30 ° C, and the dropping was added for 30 min. The solution was heated to 80 ° C and reacted for 30 min. After the reaction was completed, it was cooled to room temperature, the reaction solution was poured into 250 mL of ice water to quench, filtered, and the filter cake was recrystallized twice in anhydrous methanol to obtain needle-like crystal powder, which was collected with 2,6-dinitro-p-xylene The rate was 54.67%, and the mass fraction of HPLC analysis was 97.68%.

References:

CN111039790,2020,A Location in patent:Paragraph 0020-0024; 0032-0036; 0042-0046; 0052-0056; 0062-0