A high-yield, high-purity dast source powder synthesis process

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

Active Publication Date: 2016-04-13
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 46.565g of 4-picoline (48.66mL and 500mmol in total), 93.110g of methyl p-toluenesulfonate (75.45mL and 500mmol in total) and 63mL of absolute ethanol into the reactor, and wait until the temperature of the water bath is constant After reaching 30°C, place the reactor in a water bath to react for 24 hours, and the obtained absolute ethanol solution containing 4-methyl-N-methylpyridine p-toluenesulfonate is directly used in the second step of organic chemical reaction without treatment among.

[0015] Add all the ethanol solution containing 4-methyl-N-picoline p-toluenesulfonate, dimethylaminobenzaldehyde 74.595g (total 500mmol) prepared in the first step into another reactor, Anhydrous ethanol 265mL and catalyst di-n-butylamine 16.85mL (approximately 99.99mmol). After the temperature of the water bath was constant to 80°C, the reactor was placed in the water bath to react for 6 hours. After the reaction was completed, it was naturally cooled and allowed t...

Embodiment 2

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

[0017] Add all the ethanol solution containing 4-methyl-N-methylpyridine p-toluenesulfonate, 31.927g (total 214mmol) of dimethylaminobenzaldehyde, Anhydrous ethanol 275mL and catalyst di-n-butylamine 1.70mL (total 10.09μmol). After the temperature of the water bath was constant to 76°C, the reactor was placed in the water bath to react for 16h. The purple-red to black-purple powder precipitated in the solution. After sufficient drying, weigh and characterize the purity...

Embodiment 3

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

[0019] Add all the absolute ethanol solution containing 4-methyl-N-picoline p-toluenesulfonate and 16.409g of dimethylaminobenzaldehyde (total 109.99mmol) 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 was constant to 70 ° C, the reactor was placed in the water bath to react for 24 hours. After the reaction, it was naturally cooled ...

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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-stilbazoliumtosylate, and the Chinese name of the literal translation should be 4-N, N-dimethylamino-4'-N'-methyl - Azastilbene p-toluenesulfonate. In recent years, studies have found that the secon...

Claims

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Application Information

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Patent Type & Authority Patents(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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