Preparation method of 4-(4-dimethylaminostyryl)methylpyridyl p-toluenesulfonate

Abstract

The invention belongs to the technical field of functional material synthesis, and relates to a preparation method of 4-(4-dimethylaminostyryl)methylpyridyl p-toluenesulfonate, which comprises the following steps: mixing 4-methylpyridine and methyl-p-toluene sulfonate, putting in absolute methanol, and pouring into a three-hole flask to carry out ion-exchange reaction; dissolving dimethyl amino benzaldehyde in absolute methanol, and putting into the three-hole flask to carry out condensation reflux reaction to obtain a crystallized product; and flushing the crystallized product with trichloromethane, quickly filtering to obtain a solid with green metal luster, heating the solid with green metal luster to completely dissolve the solid in the absolute methanol, cooling, airing, and recrystallizing to obtain the 4-(4-dimethylaminostyryl)methylpyridyl p-toluenesulfonate. The preparation method has the advantages of simpleness, simple reaction steps, short reaction time, low cost and high yield.

Description

Technical field: [0001] The invention belongs to the technical field of preparation of functional materials, and relates to a process for rapidly and efficiently synthesizing 4-(4-dimethylaminostyryl)picoline p-toluenesulfonate, especially a 4-(4-dimethyl The preparation method of amino styryl) picoline p-toluene sulfonate is used to prepare high-quality organic nonlinear optical crystals. Background technique: [0002] Nonlinear optical crystals are widely used in technical and research fields. They can be made into electro-optic switches and realize laser modulation. Optical parameter oscillation can be used to achieve laser frequency tuning; some nonlinear optical effects can also be used. The phase conjugation characteristics of the nonlinear optical crystals are used for light processing; at present, the research on nonlinear optical crystals has developed into a nonlinear optical crystal material science. Actively carrying out research in this field will undoubtedly pla...

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Problems solved by technology

4-(4-Dimethylaminostyryl)picoline p-toluenesulfonate (DAST) is an organic salt crystal formed by strong Coulomb force, which has a good nonlinear optical effect, and is currently used in DAST The research is mainly focused on the realization of THz radiation through DAST crystals. 4-(4-dimethylaminostyryl)picoline p-toluenesulfonate is currently the nonlinear optical crystal with the highest THz efficiency. 4-(4 -Dimethylaminostyryl) picoline p-toluenesulfonate crystal has an asymmetric central structure, and its cation contains a benzene ring and a pyridine ring. It is a hyperconjugated ion with a large conjugated π bond, belonging to Monoclinic crystal system, the point group is m, the space group is Cc, and its unit cell parameters are: α=90°, β=92.24°, γ=90°, Z=4, although the prior art has successfully synthesized 4-(4-dimethylaminostyryl)picoline p-toluenesulfonate , but its synthesis steps are cumbersome, the yield is low, and the reaction time is long, which greatly limits the later crystal growth

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