Synthetic method of organic DSTMS crystal high-purity growth raw material

A synthesis method and organic technology, applied in the field of synthesis of high-purity organic DSTMS crystal growth raw materials, can solve the problems of reduced process cost, complex reaction process, and low product purity, and achieve the effects of low cost, simple preparation method, and simple synthesis steps

Inactive Publication Date: 2021-02-05
CHINA ELECTRONICS TECH GRP NO 46 RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for synthesizing high-purity raw materials for organic DSTMS crystal growth, which solves the problems of high cost, complex reaction process, low product purity, and difficult purification in the raw material synthesis technology, especially by self-synthesizing a synthetic process. Raw material 2,4,6-trimethylbenzenesulfonate to reduce process cost

Method used

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  • Synthetic method of organic DSTMS crystal high-purity growth raw material

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Experimental program
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Effect test

Embodiment 1

[0033] 21.87g (0.1mol) of mesitylenesulfonyl chloride was dissolved in 301mL of methanol, 1.4mL (14.13umol) of organic base piperidine was added dropwise, mixed with it, stirred, reacted at room temperature for 4 hours, and the excess solvent was removed by rotary evaporation to obtain 2 , 4,6-trimethylbenzenesulfonate; then 9.89ml (0.1mol, 9.31g) of 4-picoline and 18.65mL of 2,4,6-trimethylbenzenesulfonate (0.1mol, 21.43 g) Dissolve in 50ml of absolute ethanol successively, pour into a three-necked flask, put magnets in a water bath constant temperature magnetic stirrer, heat and stir, set the temperature at 48 ℃, condense and reflux for 8 hours, and generate an intermediate product; Finally, dissolve 14.92g (0.1mol) of p-dimethylaminobenzaldehyde in 120ml of absolute ethanol, then mix it with the intermediate product from the previous step, drop 500uL of organic base piperidine as a catalyst, and set the temperature at 75°C , reacted for 12 hours, and ended the reaction when...

Embodiment 2

[0035]Dissolve 30g (0.136mol) of mesitylenesulfonyl chloride in 410mL of methanol, add dropwise 1.8mL (18.17umol) of organic base piperidine, mix with it, stir, react at room temperature for 6 hours, remove excess solvent by rotary evaporation to obtain 2, 4,6-trimethylbenzenesulfonate; then 13.45ml (0.136mol, 12.66g) of 4-picoline and 25.36mL (0.136mol, 29.14g) of 2,4,6-trimethylbenzenesulfonate ) were successively dissolved in 68ml of absolute ethanol, poured into a three-necked flask, placed in a magnet and placed in a constant temperature magnetic stirrer in a water bath, heated and stirred, the temperature was set at 50°C, condensed and refluxed for 10 hours, and an intermediate product was generated; finally Dissolve 20.29g (0.136mol) of p-dimethylaminobenzaldehyde in 165ml of absolute ethanol, then mix it with the intermediate product from the previous step, drop 700uL of organic base piperidine as a catalyst, and set the temperature at 78°C. After 16 hours of reaction,...

Embodiment 3

[0037] 15g (0.068mol) of mesitylenesulfonyl chloride was dissolved in 205mL of methanol, 800uL (8.08umol) of organic base piperidine was added dropwise, mixed with it, stirred, reacted at room temperature for 3 hours, and the excess solvent was removed by rotary evaporation to obtain 2,4 , 6-trimethylbenzenesulfonate; then 6.73ml (0.068mol, 6.33g) of 4-picoline and 12.68mL (0.068mol, 14.57g) of 2,4,6-trimethylbenzenesulfonate Dissolved in 50ml of absolute ethanol successively, poured into a three-necked flask, placed in a magnet and placed in a constant temperature magnetic stirrer in a water bath, heated and stirred, the temperature was set at 45°C, condensed and refluxed for 8 hours, and an intermediate product was generated; finally Dissolve 14.92g (0.068mol) of p-dimethylaminobenzaldehyde in 100ml of absolute ethanol, then mix it with the intermediate product from the previous step, drop 500uL of organic base piperidine as a catalyst, set the temperature at 70°C, and react ...

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Abstract

The invention discloses a synthetic method of an organic DSTMS crystal high-purity growth raw material. The method comprises the following steps of: 1, reacting mesitylene sulfonyl chloride and methanol serving as reactants and organic alkali piperidine serving as an acid-binding agent at room temperature to obtain 2, 4, 6-trimethylbenzenesulfonate; 2, dissolving 4-methylpyridine and the 2, 4, 6-trimethylbenzenesulfonate in absolute ethyl alcohol, and carrying out condensation reflux reaction to generate an intermediate product 4-methyl-N-methylpyridine- 2, 4, 6-trimethylbenzenesulfonate; and3, mixing p-dimethylaminobenzaldehyde with the intermediate product generated by the reaction by taking absolute ethyl alcohol as a solvent and organic alkali piperidine as a catalyst, putting the mixture into a stirrer, stirring, condensing, refluxing and reacting to finally obtain the DSTMS raw material. The DSTMS raw material synthesis process provided by the invention has the advantages of high yield, high purity, low cost and simple steps. Through adjustment of technological parameters, the DSTMS raw material with the yield of 75%-89% and the purity of 90-96% is finally obtained.

Description

technical field [0001] The invention relates to a raw material synthesis method of 4-(4-dimethylaminostyryl)picoline p-toluenesulfonate (DAST) derivatives of organic crystal material. In particular, it relates to a high-purity, high-yield, low-cost, and simple synthesis method for the synthesis of organic DSTMS crystal high-purity growth raw materials. Background technique [0002] Terahertz (THz) wave is an electromagnetic wave between microwave and infrared light. It occupies a special position in the spectrum and has important research value. Terahertz radiation has the characteristics of strong penetrability, wide bandwidth, and small damage. Based on these advantages, terahertz technology is widely used in terahertz imaging, terahertz communication, terahertz time-domain spectroscopy and other fields. Organic nonlinear optics (NLO) crystals are ideal materials for THz radiation sources, which can generate THz waves by optical rectification (OR) and difference frequenc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/20C07D213/127C07C303/32C07C303/44C07C309/30C07C303/28C07C309/73
CPCC07D213/20C07D213/127C07C303/32C07C303/44C07C303/28C07B2200/13
Inventor 王健孟欢徐世海庞子博李瑜萍程红娟李宝珠
Owner CHINA ELECTRONICS TECH GRP NO 46 RES INST
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