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High-yield high-purity DAST source powder synthetic process

A synthetic process and high-purity technology, applied in organic chemistry and other fields, can solve problems such as low yield and difficult product purification, and achieve the effect of reducing pollution

Active Publication Date: 2015-02-11
CHINA ELECTRONICS TECH GRP NO 46 RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of the existing DAST source powder synthesis technology, such as the use of toxic and harmful solvents, low yield, and difficult product purification. In particular, it provides a "green solvent" as a reaction solvent, through two-step organic chemical reactions, successfully Realize a high-yield, high-purity DAST source powder synthesis process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Add 46.565 g of 4-picoline (together 48.66 mL and 500 mmol), 93.110 g of methyl p-toluenesulfonate (total of 75.45 mL and 500 mmol) and 63 mL of absolute ethanol into the reactor, and wait in a water bath After the temperature of the pot was kept constant to 30 °C, the reactor was placed in a water bath to react for 24 h, and the obtained absolute ethanol solution containing 4-methyl-N-methylpyridine p-toluenesulfonate was directly used in the second step in an organic chemical reaction.

[0015] Add all the ethanol solution containing 4-methyl-N-picoline p-toluenesulfonate, 74.595g (total 500mmol) of dimethylaminobenzaldehyde, 265 mL of absolute ethanol and 16.85 mL of di-n-butylamine (about 99.99 mmol) as the catalyst. After the temperature of the water bath was constant to 80 °C, the reactor was placed in the water bath to react for 6 h. After the reaction, it was naturally cooled and statically Set aside, collect the purple-red to black-purple powder pre...

Embodiment 2

[0016] Example 2: Add 19.557 g of 4-picoline (together 20.44 mL and 210 mmol), 37.244 g of methyl p-toluenesulfonate (together 30.18 mL and 200 mmol) and 100 mL of absolute ethanol into the reactor, and wait for the water bath After the temperature of the pot was kept constant to 50°C, the reactor was placed in a water bath to react for 12 hours, and the obtained absolute ethanol solution containing 4-methyl-N-picoline p-toluenesulfonate was directly used in the second step without treatment in organic chemical reactions.

[0017] Add all the absolute ethanol solution containing 4-methyl-N-picoline p-toluenesulfonate and 31.927g (together 214 mmol) of dimethylaminobenzaldehyde prepared in the first step into another reactor , 275mL of absolute ethanol and 1.70mL of catalyst di-n-butylamine (total 10.09 μmol). After the temperature of the water bath was constant to 76°C, the reactor was placed in the water bath for 16 hours of reaction. The purple-red to black-purple powder pr...

Embodiment 3

[0018] Example 3: Add 10.244 g of 4-picoline (about 10.70 mL and 110 mmol), 18.622 g of methyl p-toluenesulfonate (about 15.09 mL and 100 mmol) and 154 mL of absolute ethanol into the reactor, and wait After the temperature of the water bath was kept constant to 70 °C, the reactor was placed in the water bath for 3 h, and the obtained absolute ethanol solution containing 4-methyl-N-methylpyridine p-toluenesulfonate was directly used in the second stage without treatment. Two-step organic chemical reaction.

[0019] Add all the absolute ethanol solution containing 4-methyl-N-methylpyridine p-toluenesulfonate and 16.409g of dimethylaminobenzaldehyde (total 109.99 mmol) prepared in the first step into another reactor , 780 mL of absolute ethanol and 170 μL of catalyst di-n-butylamine (total 1.01 mmol), after the temperature of the water bath is constant to 70°C, place the reactor in the water bath for 24 hours of reaction, after the reaction is completed, cool naturally and let s...

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Abstract

The invention discloses a high-yield high-purity DAST source powder synthetic process. The synthetic process comprises the following two steps: 1, reacting 4-methylpyridine with methyl p-toluenesulfonate in the presence of absolute ethyl alcohol serving as a solvent to obtain an absolute ethyl alcohol solution of 4-methyl-N-methylpyridine tosilate; and 2, reacting 4-methyl-N-methylpyridine tosilate with p-dimethylaminobenzaldehyde in the presence of absolute ethyl alcohol serving as a solvent and under the catalytic action of di-n-butylamine or piperidine, so as to obtain high-yield (85-95%) high-quality (90-95%) DAST source powder. According to the synthetic process, absolute ethyl alcohol is used as a reaction solvent, harm of poisonous and harmful solvents such as methylbenzene and methyl alcohol to the body of an operator can be avoided and the pollution of waste liquid to the environment can be avoided. The research success of the high-yield high-purity DAST source powder synthetic process is beneficial to culture of high-quality large-sized DAST crystal, thereby laying a good material and theoretical basis for research on the DAST crystal and related products.

Description

technical field [0001] The present invention relates to the preparation method of DAST (4-N, N-dimethylamino-4'-N'-methyl-azastilbene p-toluenesulfonate) source powder, in particular to a high-yield, high-purity DAST source powder synthesis process. Background technique [0002] Due to the advantages of large nonlinear optical coefficient, fast response speed, high resistance to photodamage threshold, low dielectric constant, and easy molecular design, organic nonlinear optical materials have attracted the attention of researchers in the fields of chemistry, crystallography, and optics. Among them, S. R. Marder et al first reported the DAST crystal with second-order optical nonlinearity in August 1989. DAST is the abbreviation of its English name 4-N, N-dimethylamino-4'-N'-methyl-stilbazolium tosylate, and the Chinese name of the literal translation should be 4-N, N-dimethylamino-4'-N'-methyl Base-azastilbene p-toluenesulfonate. In recent years, studies have found that th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/38
CPCC07D213/38
Inventor 庞子博孟大磊马思睿窦瑛程红娟洪颖徐永宽
Owner CHINA ELECTRONICS TECH GRP NO 46 RES INST
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