Synthesis method of spirodiclofen

Abstract

The invention discloses a synthesis method of spirodiclofen. The synthesis method comprises the following steps: enabling 3-(2,4-dichlorophenyl)-2-oxo-1-oxaspiro[4,5]-deca-3-ene4-ol and 2-2-dimethylbutyl chloride serving as raw materials to have a reaction in the presence of triethylamine serving as a catalyst in a non-proton type organic solvent; after the reaction is over, regulating the pH value of the reaction liquid to 10-11 with alkali liquid, standing for layering to obtain an aqueous phase and an organic phase, and separating out the aqueous phase as the alkali liquid in next batch of synthesis; washing the organic phase with water, drying with anhydrous sodium sulfate, heating and performing atmospheric distillation to remove a mixed solvent containing triethylamine and the non-proton type organic solvent, so as to obtain a solid product, wherein the removed mixed solvent is used as the catalyst and non-proton type organic solvent in next batch of synthesis; and recrystallizing the obtained solid product to obtain the product spirodiclofen. Triethylamine and dichloromethane are recovered together and directly utilized in next batch of synthesis, so that the production cost is lowered, and the emission of high-concentration brine waste water can be reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis method of spirodiclofen. Background technique [0002] Spirodiclofen (mite danger) was originally a spirotetronic acid insecticide and acaricide developed by Bayer. It has been used to control whitefly and spider mites on cotton, vegetables, citrus, pome fruit, grapes and other crops. Harmful mites. As a miticide with a new mechanism of action developed by Bayer CropScience for more than ten years, its miticide mechanism is completely different from the existing various miticides. Spirodifen inhibits the fat synthesis in the body of harmful mites, destroys the energy metabolism activities of the mites, and finally kills the harmful mites. It is a brand-new, high-efficiency non-systemic foliar treatment acaricide. There is no cross-resistance problem, and it has good control effect and excellent persistent effect on different acarids of various crops. It...

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Problems solved by technology

The disadvantage is that it adopts the method of heating and distilling industrial waste water into a strong base. The amount of industrial production waste water is usually large. Directly heating and distilling the waste water requires a large amount of steam, and the production cost is very high. Moreover, after triethylamine and toluene are distilled, Other organic matter and salt impurities in the wastewater need to be further treated, and this method is costly in industrial production

At the same time, it first steams the mixed solution of triethylamine, toluene and water in the wastewater, and then adds calcium oxide to reflux for 48 minutes to dry, which also requires heating and increases the production cost; after drying, the mixed solution is transferred to another flask , to purify triethylamine and toluene

This step needs to transfer the mixed liquid, which increases the operation steps. In industrial production, it is necessary to cool the hot material and then transfer it to another reactor, and then heat up and distill, which further increases the production cost and operation steps.

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