Synthesis method of 2-acetonyl-1, 4-dimethyl succinate

A technology for the synthesis of dimethyl succinate and a synthesis method, which is applied in the field of synthesis of 2-acetonyl-1,4-dimethyl succinate, and can solve problems such as high reaction temperature, large amount of catalyst, and long reaction time , to achieve the effects of simple reaction system, easy post-treatment operation, and cheap raw materials

Pending Publication Date: 2022-03-15
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

This technology simplifies the process by making it easier or simpler than existing methods that require expensive chemicals. It also makes manufacturing processes more efficient because they don't have complex steps like extra cleaning needed after each use.

Problems solved by technology

This patented technical problem addressed by this patents relates to improving the efficiency and productivity of chemical reactions used during manufacturing processes like dialkoxymers or polycondensation chemistry.

Method used

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  • Synthesis method of 2-acetonyl-1, 4-dimethyl succinate
  • Synthesis method of 2-acetonyl-1, 4-dimethyl succinate
  • Synthesis method of 2-acetonyl-1, 4-dimethyl succinate

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Embodiment 1

[0024] A kind of 2-acetonyl-1,4-succinic acid dimethyl ester synthetic method, described synthetic method is as follows:

[0025] Acetone (93.10g, 1.6mol), dimethyl maleate (28.87g, 0.2mol) and pyrrolidine (2.84g, 0.04mol) were successively added into a 250mL three-necked flask equipped with a thermometer and a reflux condenser, at 40 Reaction at ℃ for 12 hours; after the reaction, distill the remaining unreacted acetone from the reaction solution at 60℃, acidify to adjust the pH to 1, extract with ethyl acetate, take the organic layer and evaporate the solvent, then under 2-5mmHg vacuum Fractions at 70-100°C were collected to obtain 28.6 g of light yellow liquid with a yield of 70.6%.

Embodiment 2

[0027] A kind of 2-acetonyl-1,4-succinic acid dimethyl ester synthetic method, described synthetic method is as follows:

[0028] Acetone (92.93g, 1.6mol), dimethyl maleate (28.80g, 0.2mol) and pyrrolidine (2.84g, 0.04mol) were successively added into a 250mL three-necked flask equipped with a thermometer and a reflux condenser, at 60 Reaction at ℃ for 12 hours; after the reaction, distill the remaining unreacted acetone from the reaction solution at 60℃, acidify to adjust the pH to 1, extract with ethyl acetate, take the organic layer and evaporate the solvent, then under 2-5mmHg vacuum Fractions at 70-100°C were collected to obtain 28.9 g of light yellow liquid with a yield of 71.5%.

Embodiment 3

[0030] A kind of 2-acetonyl-1,4-succinic acid dimethyl ester synthetic method, described synthetic method is as follows:

[0031] Acetone (92.94g, 1.6mol), dimethyl maleate (28.91g, 0.2mol) and pyrrolidine (2.83g, 0.04mol) were sequentially added into a 250mL autoclave, and reacted at 140°C for 12h; the reaction was completed Finally, the remaining unreacted acetone was evaporated from the reaction solution at 60°C, acidified to adjust the pH to 2, extracted with ethyl acetate, the organic layer was taken to remove the solvent, and then the fraction at 70-100°C was collected under a vacuum of 2-5 mmHg. 26.6 g of light yellow liquid was obtained, the yield was 65.6%.

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Abstract

The invention discloses a synthesis method of 2-acetonyl-1, 4-dimethyl succinate, which comprises the following steps: mixing acetone (1), dimethyl maleate (2) and pyrrolidine, reacting at 20-200 DEG C for 0.5-20 hours, and post-treating the reaction liquid to obtain 2-acetonyl-1, 4-dimethyl succinate (3); the reaction system is simple, raw materials are cheap and easy to obtain, post-treatment operation is simple and convenient, and industrial production is facilitated;

Description

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Claims

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Application Information

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Owner ZHEJIANG UNIV OF TECH
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