121results about How to "The post-processing method is simple" patented technology

The invention relates to a method for preparing 2-amino-4,6-dichloro-5-formamido pyrimidine. The method comprises the following steps of: performing nitrosation on malonic acid diethyl ester and acetic acid serving as raw materials and sodium nitrite at first; then, performing reduction and formylation with formic acid in the presence of zinc powder to form formyl amino malonic acid diethyl ester; finally, performing condensation and cyclization with guanidine hydrochloride to produce 2-amino-4,6-dichloro-5-formamido pyrimidine; performing chlorination by using quaternary ammonium salt as a catalyst; fractionally performing hydrolysis under an alkali action to obtain a product. The method has easily-available raw materials, and is short in reaction time, simple in aftertreatment and high in hydrolysis selectivity; the cost is obviously reduced; the total yield is up to 74 percent and the purity of the product is up to 99.0 percent.

The invention relates to a preparation method of a prothioconazole intermediate. The preparation method comprises the following steps: dissolving [1-(2-chlorophenyl)-2-(1-chlorocyclopropyl)-2-hydroxy]-propyl hydrazine into methyl benzene; dropwise adding a formaldehyde aqueous solution or a polyformaldehyde aqueous solution under 30 to 35 DEG C; then adding in thiocyanate after completion of dropwise adding; then dropwise adding hydrochloric acid or sulfuric acid aqueous solution; keeping warm and reacting for 50 to 70 minutes after completion of dropwise adding; directly using a reaction solution for follow-up reaction or filtering the reaction solution after cooling; thus obtaining the prothioconazole intermediate 2-(1-chloro-cyclopropyl-1-yl)-1-(2-chlorophenyl)-2-hydroxy-3-(1,2,4-triazolidine-5-thioketone-1-yl)-propane. Through optimization on a whole route, for example, reaction temperature, reagents, a feeding procedure and the like, of the preparation method, an after-treatment method is simple, three wastes such as waste gas, waste water and waste residues are few, the reaction time is shortened, the purity and the yield of a product are higher, and the preparation method is suitable for industrial production.