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Preparation method of dimethyl succinyl succinate

A technology of dimethyl succinyl succinate and dimethyl succinate, applied in the field of preparation of dimethyl succinyl succinate, can solve the problems of unsatisfactory improvement of production efficiency and quality, etc. Achieve the effects of improving synthesis efficiency, simple preparation process, and high purity of finished products

Active Publication Date: 2021-02-23
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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  • Preparation method of dimethyl succinyl succinate
  • Preparation method of dimethyl succinyl succinate
  • Preparation method of dimethyl succinyl succinate

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preparation example Construction

[0021] The present embodiment provides a kind of preparation method of dimethyl succinyl succinate, such as Figure 2~3 As shown, it includes the following steps: S10 Adding methanol solution of dimethyl succinate into the reactor, heating to 60±1° C., and keeping the temperature for 15-30 minutes to obtain the first mixed solution. S20 Add dropwise a methanol solution of 1,8-diazacyclo[5,4,0]undecene-7 (DBU) into the first mixed solution, and obtain a second mixed solution after the dropwise addition is completed. S30 raising the temperature of the second mixed solution to 80-140° C., and reacting for 2-3 hours to complete the reaction to obtain a third mixed solution. and S40, reducing the third mixed solution to 80° C. for distillation, and cooling to room temperature to obtain dimethyl succinyl succinate as a solid.

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

Embodiment 1

[0026] S10 Add 29.23g of dimethyl succinate (manufactured by Sinopharm) and 100ml of anhydrous methanol solution to a 500ml four-neck flask respectively, heat up to 60°C while stirring, and keep for 15min to obtain the first mixed solution.

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

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

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

Embodiment 2

[0031] S10 Add 70 kg of dimethyl succinate (manufactured by Changzhou Xiaqing Technology Co., Ltd., purity> 98%) and 100 kg of anhydrous methanol solution into the reaction kettle respectively, stir while raising the temperature to 60° C., and keep it for 25 minutes to obtain the first mixture.

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

[0033] S30 pressurizes and raises the temperature of the second mixed solution to 140° C., and reacts for 3 hours to complete the reaction to obtain a third mixed solution.

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

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Abstract

The invention provides a preparation method of dimethyl succinyl succinate, which comprises the following steps: S10, adding a methanol solution of dimethyl succinate into a reactor, heating to 60+ / -1DEG C, and keeping the temperature for 15-30 minutes to obtain a first mixed solution, S20, dropwise adding a methanol solution of 1, 8-diazacyclo[5, 4, 0]undecen-7 (DBU) into the first mixed solution, and obtaining a second mixed solution after dropwise adding is finished, S30, heating the second mixed solution to 80-140 DEG C, and carrying out a reaction for 2-3 h to complete the reaction so asto obtain a third mixed solution, and S40, cooling the third mixed solution to 80 DEG C, distilling, and cooling to room temperature to obtain a dimethyl succinyl succinate solid. According to the preparation method of dimethyl succinyl succinate, DBU is adopted as a catalyst, dimethyl succinate and methanol are directly reacted to synthesize dimethyl succinyl succinate, the preparation process is simple, the yield of the synthesized product is greater than 94%, and the synthesis efficiency is greatly improved.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of dimethyl succinylsuccinate. Background technique [0002] Dimethyl succinyl succinate (DMSS) is an important intermediate in organic synthesis, and it is the main raw material for the preparation of high-grade organic pigments of quinacridones. Such as high-grade pigment red 122. Pigment Red 122 is a kind of high-performance organic pigment. The pigment has bright color, good heat resistance to organic solvents, excellent light fastness 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 coloring of synthetic fibers, and can also be blended with other pigments. Its common synthetic route is as follows figure 1 shown. [0003] The invention patent of notification number CN108373412A discloses a method for continuous pr...

Claims

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Application Information

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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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