A preparation method of thieno[3,4-b]-1,4-dioxin-2-methanol derivatives

Abstract

The invention discloses a preparation method of thieno[3,4-b]-1,4-dioxin-2-methanol derivatives, comprising the following steps: S1, adding a first reaction solvent and raw materials into a three-necked flask Thieno[3,4-b]-1,4-dioxin-2-methanol, the first reactant, and a catalyst to obtain the first mixed solution; S2, adding the alkali solution dropwise; S3, obtaining the first mixture after the reaction Reaction solution; S4, standing the first reaction solution for stratification to obtain an organic phase and an extract; S5, merging the organic phase and the extract, and drying; S6, filtering and drying to obtain an intermediate product; S7, in a three-necked flask Adding a second reaction solvent and an intermediate product to obtain a mixed solution; S8, concentrating the mixed solution; S9, adding an alkali solution dropwise; S10, extracting and collecting the organic phase; S11, washing the organic phase with water; S12, drying the organic phase , concentrating to obtain a second mixture; S13, eluting and drying the second mixture to obtain the target product.

Description

Technical field [0001] The present invention relates to the field of preparing the compounds, and in particular [3,4-b] -1,4- dioxin-2-methanol derivative relates to a method of thiophene Background technique [0002] The name of the desired product 3 - [(2,3-dihydro-thieno [3,4-b] -1,4- dioxin-2-yl) methoxy] - propionic acid, 3,4-ethylenedioxythiophene dioxythiophene (abbreviation of EDOT) derivatives. EDOT monomer is a conducting polymer Bayer discovered, which belongs to the electronic chemicals. The desired product is stable conductive compound monomer, is the basic material of the conductive skeleton, can be prepared by condensation of carboxylic acid esters is further applied to lithium battery electrolyte. Desired product in the prior art only a synthesis route (e.g. figure 1 Shown), it was found during the synthesis, the synthesis of low product yield, and was used in the reaction of 3-bromo - propionate having photosensitivity, see light easily degradable, easily treated...

AI Technical Summary

Problems solved by technology

The target product has only one synthetic route in the prior art (such as figure 1 shown), but found in the synthesis process that the yield of the finished product of the synthesis process is low, and the reactant 3-bromo-ethyl propionate used has photosensitivity, is easily degraded when exposed to light, and is not easy to handle. Sodium hydride is chemically active and can spontaneously ignite in humid air. It has great safety hazards in industrial production. Therefore, it is necessary to seek a new synthesis process to prepare the target product

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