Synthesis method of alpha,gamma,gamma,gamma-tetrachlorobutyrate

Abstract

The invention relates to a synthesis method of alpha,gamma,gamma,gamma-tetrachlorobutyrate. The synthesis method comprises the following steps: stirring and mixing carbon tetrachloride and acrylate with a copper salt and / or cuprous salt main catalyst, an organic amine or imidazole cocatalyst and a polar inert organic solvent at room temperature, sealing a reaction kettle, conducting heating for anaddition reaction, preforming cooling to room temperature, carrying out filtering, distilling a filtrate under normal pressure to recover carbon tetrachloride, and performing rectifying under reducedpressure to obtain alpha,gamma,gamma,gamma-tetrachlorobutyrate. The purity of the alpha,gamma,gamma,gamma-tetrachlorobutyrate obtained by using the method is up to 99.5%, one-way reaction yield is upto 96.1%, a product is easy to separate, reaction byproducts are few, the catalytic effect of the catalysts and the ligand is excellent, the raw materials and the catalysts are cheap and easy to obtain, and the solvent and the catalysts are easy to recycle; and the method is mild in reaction condition, simple in technological operation, low in production cost, good in economic benefit and suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis method of α, γ, γ, γ-tetrachlorobutyrate, in particular to a synthesis method of (α-methyl)-α, γ, γ, γ-tetrachlorobutyrate. Background technique [0002] (α-Methyl)-α,γ,γ,γ-Tetrachlorobutyrate is an important class of raw materials for organic synthesis and an important initiator in the synthesis of acrylic resins. It is used in the synthesis of fine chemicals It also has more important uses; it has broad application prospects in the field of pesticide synthesis, especially in the synthesis of chlorinated pyrethroid compounds. As we all know, chlorine is one of the commonly used highly active non-metallic elements. Based on its nuclear structure characteristics, it has strong reaction advantages in terms of electronegativity and bond energy. Many properties such as anti-corrosion and anti-corrosion have been strengthened. Therefore, (α-methyl)-α,γ,γ,γ-tetrachlorobutyrate has great development potential in the new ...

AI Technical Summary

Problems solved by technology

However, the yield of synthesizing α, γ, γ, γ-methyl tetrachlorobutyrate with methyl acrylate as the basic raw material is only 47%; the synthesis of α-methyl-α, γ , The yield of γ, γ-tetrachlorobutyric acid methyl ester is only 66%, and the preparation method of the catalyst tris (2-pyridylmethyl) amine-copper complex is complex, the reaction operation is cumbersome, and the reaction by-product components are complex, high There are many boiling point multi-focus oils, which are difficult to post-process and are not suitable for industrial applications (Dalton Trans., 2011, 40, 3060-3066)

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