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Synthetic method of dimethyl succinyl succinate

A technology of dimethyl succinyl succinate and dimethyl succinate, which is applied in the field of synthesis of dimethyl succinyl succinate, can solve the problem of affecting product yield and purity, increasing production costs, and raw materials. Loss and other issues, to achieve the effect of high product yield, easy recycling, and stable quality

Active Publication Date: 2020-12-18
河北彩客新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the improved process route has improved product yield and shortened reaction time, excessive dimethyl succinate is prone to side reactions, and dimethyl succinate is easily hydrolyzed during high-temperature polymerization and acidification Cause loss of raw materials, which in turn affects product yield and purity, and increases production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of synthetic method of dimethyl succinyl succinate, comprises the steps:

[0023] Add 73g (0.5mol) of dimethyl succinate and 210g of liquid paraffin to a 500ml four-neck flask equipped with a stirring device, a thermometer and a distillation device, and under nitrogen protection, heat up to 135°C while stirring, and start to drop 94.5g (0.525mol) of sodium methoxide methanol solution (30wt%) was added dropwise for 2 hours. After the dropwise addition was completed, the temperature was raised to 140° C. and kept for 1.5 hours of reaction.

[0024] After the reaction, cool down to 50°C, add sulfuric acid solution with a concentration of 30% to adjust the pH of the reaction system to about 2 for acidification, stir at 45°C for 0.5h, retest the pH value to 2, and filter the reaction solution with suction. The resulting filter cake was washed with water and dried to obtain 48.3 g of dimethyl succinyl succinate with a yield of 84.66%, a purity of 99.61% (HPLC), and a m...

Embodiment 2

[0026] A kind of synthetic method of dimethyl succinyl succinate, comprises the steps:

[0027] Add 73g (0.5mol) of dimethyl succinate and 219g of liquid paraffin to a 500ml four-neck flask equipped with a stirring device, a thermometer and a distillation device, and under nitrogen protection, heat up to 140°C while stirring, and start to drop 94.5g (0.525mol) of sodium methoxide methanol solution (30wt%) was added dropwise for 2.5 hours. After the dropwise addition was completed, the temperature was raised to 145° C. for 0.5 hours of reaction.

[0028] After the reaction, cool down to 50°C, add sulfuric acid solution with a concentration of 30% to adjust the pH of the reaction system to about 2 for acidification, stir at 45°C for 0.5h, retest the pH value to 2, and filter the reaction solution with suction. The resulting filter cake was washed with water and dried to obtain 48.9 g of dimethyl succinyl succinate with a yield of 85.71%, a purity of 99.59% (HPLC), and a melting ...

Embodiment 3

[0030] A kind of synthetic method of dimethyl succinyl succinate, comprises the steps:

[0031] Add 73g (0.5mol) of dimethyl succinate and 233g of liquid paraffin into a 500ml four-neck flask equipped with a stirring device, a thermometer and a distillation device, and under nitrogen protection, heat up to 137°C while stirring, and start to drop 99.0g (0.55mol) of sodium methoxide methanol solution (30wt%) was added dropwise for 2 hours. After the dropwise addition, the temperature was raised to 140° C. and kept for reaction for 1.5 hours.

[0032] After the reaction, cool down to 45°C, add 30% sulfuric acid solution to adjust the pH of the reaction system to about 2 for acidification, stir at 45°C for 0.5h, retest the pH value to 2, and filter the reaction solution with suction. The resulting filter cake was washed with water and dried to obtain 48.8 g of dimethyl succinosuccinate with a yield of 85.54%, a purity of 99.63% (HPLC), and a melting point of 154.9 to 156.1°C; The...

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Abstract

The invention relates to the technical field of organic synthesis, and particularly discloses a synthetic method of dimethyl succinyl succinate. The synthesis method comprises the following steps: taking liquid paraffin as a reaction solvent and dimethyl succinate as a raw material to react with sodium methoxide, and performing acidification treatment, suction filtration, washing and drying to obtain the dimethyl succinyl succinate. According to the synthetic method of dimethyl succinyl succinate, liquid paraffin is adopted to replace dimethyl succinate to serve as a reaction solvent, the problems that excessive dimethyl succinate is prone to side reaction and prone to hydrolysis in the high-temperature polymerization and acidification process to cause loss of raw materials are effectivelysolved. Besides, the yield and purity of the dimethyl succinyl succinate product are guaranteed, the average yield of the product is 85.54%, the purity of the product is 99.5% or above, and the product quality is stable.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing dimethyl succinylsuccinate. Background technique [0002] Dimethyl succinyl succinate (DMSS) is an important intermediate for the preparation of quinacridone pigments. There are many synthesis techniques for this compound, and the basic process route is to use dimethyl succinate in an inert solvent through the action of sodium alkoxide to undergo self-condensation to generate dimethyl succinyl succinate. Commonly used solvents include xylene, toluene, chlorobenzene, etc., and a small amount of polar co-solvent is often added to promote the reaction. Common polar cosolvents include dimethyl sulfoxide, dimethylformamide, sulfolane, etc. No matter what kind of mixed solvent composed of inert solvent and co-solvent is used, there is a common disadvantage, that is, the reaction time is long, the product separation and purification process is compl...

Claims

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Application Information

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IPC IPC(8): C07C67/313C07C67/343C07C69/757
CPCC07C67/313C07C67/343C07C2601/14C07C69/757
Inventor 王淑梅王朝聘李祥金韩红霞张金月张吉晔崔北文刘子洋
Owner 河北彩客新材料科技股份有限公司
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