202842-98-6Relevant articles and documents
Preparation method of 3, 4-dimethylpyrazole and phosphate thereof
-
Paragraph 0054; 0058-0059; 0063-0064; 0068-0069; 0073, (2021/02/06)
The invention discloses a preparation method of 3, 4-dimethylpyrazole and phosphate thereof, which comprises the following steps: S1. making 2-butanone react with formate at -10 to 50 DEG C in a reaction solvent under the condition of keeping alkaline by using an alkaline substance, carrying out extraction separation, adding an alkylation reagent, continuing the reaction to obtain a reaction solution, and carrying out post-treatment to obtain a solution of an alkene ether compound, and S2, making the alkene ether compound prepared in the step S1 react with hydrazine hydrate or hydrazine salt at the temperature of -10 to 60 DEG C after the pH value is adjusted to 2-9, adding the alkaline substance to adjust the pH value to 7-11 after the reaction is finished, and carrying out post-treatmentto obtain the 3, 4-dimethyl pyrazole. The preparation method disclosed by the invention has the remarkable advantages of cheap raw materials, simplicity and convenience in operation, high yield, simplicity in three-waste treatment, high product quality, capability of recycling the solvent and the like, and is suitable for industrial production.
Method for preparing 3, 4-dimethylpyrazole and phosphate thereof
-
Paragraph 0103; 0104; 0110; 0111; 0119; 0127, (2019/04/17)
The invention discloses a method for preparing 3, 4-dimethylpyrazole and phosphate thereof. The method for preparing the 3, 4-dimethylpyrazole includes the steps: (1) feeding 2-butanone, aldehyde andalkali solution into a microchannel reactor and performing aldehyde ketone condensation reaction to produce 4-hydroxy-3-methyl-2-butanone salt; (2) mixing reaction liquid obtained in the step (1) andacid liquid in the microchannel reactor to obtain 4-hydroxy-3-methyl-2-butanone water solution; (3) performing reaction on hydrazine hydrate and the 4-hydroxy-3-methyl-2-butanone water solution in themicrochannel reactor, mixing reaction liquid with the alkali solution and hydrogen peroxide, and performing oxidative dehydrogenation reaction to obtain 3, 4-dimethylpyrazole water solution; (4) performing organic extraction and distillation on the 3, 4-dimethylpyrazole water solution to obtain the 3, 4-dimethylpyrazole. According to the method, reaction time is greatly shortened, the yield and the purity of products are ensured, and continuous production can be realized.