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A kind of preparation method of dimethyl succinyl succinate

A technology of dimethyl succinyl succinate and dimethyl succinate is applied in the field of preparation of dimethyl succinyl succinate, and can solve the problems of unsatisfactory improvement effect of preparation efficiency and quality, and the like, Achieve the effect of improving synthesis efficiency, high purity of finished product and simple preparation process

Active Publication Date: 2022-08-09
江苏苏御新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the method disclosed in this invention, the improvement effect of product preparation efficiency and quality is not ideal

Method used

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  • A kind of preparation method of dimethyl succinyl succinate
  • A kind of preparation method of dimethyl succinyl succinate
  • A kind of preparation method of dimethyl succinyl succinate

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preparation example Construction

[0021] The present embodiment provides a preparation method of dimethyl succinyl succinate, such as Figures 2 to 3 As shown, the following steps are included: S10, adding methanol solution of dimethyl succinate to the reactor, heating to 60±1° C., and maintaining the temperature for 15-30 minutes to obtain a first mixed solution. S20 Add dropwise a methanol solution of 1,8-diazacyclo[5,4,0]undecene-7 (DBU) to the first mixed solution, and after the dropwise addition is completed, a second mixed solution is obtained. S30, the temperature of the second mixed solution is raised to 80-140° C., and the reaction is completed for 2-3 hours to obtain a third mixed solution. and S40, the third mixed solution is lowered to 80° C. for distillation, and cooled to room temperature to obtain a solid of dimethyl succinyl succinate.

[0022] Claisen condensation reaction refers to the reaction in which ester containing α-hydrogen undergoes condensation under the action of a basic condensing...

Embodiment 1

[0026] S10 29.23g of dimethyl succinate (produced by Sinopharm Group) and 100ml of anhydrous methanol solution were added to a 500ml four-necked flask respectively, and the temperature was raised to 60°C while stirring, and kept for 15min to obtain the first mixed solution.

[0027] S20 Drop 50 ml of a methanol solution of DBU with a mass fraction of 0.58% into the first mixed solution, and after the dropwise addition is completed, a second mixed solution is obtained.

[0028] S30, the temperature of the second mixed solution is raised to 80° C., and the reaction is completed for 2 hours to obtain a third mixed solution.

[0029] S40 Distill the third mixed solution at 80° C., collect the distilled DBU and methanol mixed solution, and cool the remaining solution to room temperature to obtain 21.7 g of solid dimethyl succinyl succinate with a yield of 95%.

Embodiment 2

[0031] S10 Add 70kg of dimethyl succinate (produced by Changzhou Xiaqing Technology Co., Ltd., purity > 98%) and 100kg of anhydrous methanol solution in the reaction kettle respectively, while stirring, the temperature is raised to 60 ° C and kept for 25min to obtain the first mixture.

[0032] S20 Drop 10 kg of a methanol solution of DBU with a mass fraction of 7% into the first mixed solution, and after the dropwise addition is completed, a second mixed solution is obtained.

[0033] In S30, the second mixed solution is pressurized and heated to 140° C., and the reaction is completed for 3 hours to obtain a third mixed solution.

[0034] S40 Distill the third mixed solution at 80° C., collect the distilled DBU and methanol mixed solution, and cool the remaining solution to room temperature to obtain 51.8 kg of solid dimethyl succinyl succinate with a yield of 94.96%.

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Abstract

The invention provides a method for preparing dimethyl succinate, which includes the following steps: S10: add a methanol solution of dimethyl succinate into the reactor, heat it to 60±1°C, and keep it warm for 15 to 30 Minutes, obtain the first mixed solution; S20 dropwise add the methanol solution of 1,8-diazacyclo[5,4,0]undecene-7 (DBU) into the first mixed solution, after the addition is completed , obtain the second mixed solution; S30, heat the second mixed solution to 80-140°C, react for 2-3 hours to complete the reaction, and obtain the third mixed solution; and S40, lower the third mixed solution to 80°C for distillation , cooled to room temperature, and obtained dimethyl succinylsuccinate solid. The preparation method of dimethyl succinate of the present invention uses DBU as a catalyst and directly reacts dimethyl succinate with methanol to synthesize dimethyl succinate. The preparation process is simple and the synthesis is The product yield is greater than 94%, which greatly improves the synthesis efficiency.

Description

Technical field [0001] The invention relates to the technical field of chemical synthesis, and in particular to a preparation method of dimethyl succinylsuccinate. Background technique [0002] Dimethyl succinate (DMSS) is an important organic synthesis intermediate and the main raw material for the preparation of high-grade quinacridone organic pigments. Such as high-end pigment red 122. Pigment Red 122 is a type of high-performance organic pigment. The pigment has bright color, good heat resistance to organic solvents, excellent light resistance and weather resistance, and does not migrate in various plastics. It is mainly used in plastics and coatings. , resin, printing, ink, textile, rubber coloring, also used for the puree coloring of synthetic fibers, and can also be mixed with other pigments. Its common synthesis routes are as follows: figure 1 shown. [0003] The invention patent with announcement number CN108373412A discloses a method for the continuous producti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/313C07C67/343C07C67/52C07C69/757
CPCC07C67/313C07C67/343C07C67/52C07C2601/14C07C69/757
Inventor 张晓明
Owner 江苏苏御新材料科技有限公司
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