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Synthetic method of ethyl ethoxy acrylate

A technology of ethyl ethoxy acrylate and a synthesis method is applied in the field of synthesizing ethyl ethoxy acrylate, can solve problems such as being unsuitable for industrialized production, cumbersome operations, long steps, etc., and achieves obvious competitive advantages and cheap and easy-to-obtain raw materials , the effect of low production cost

Active Publication Date: 2014-08-06
ZHEJIANG BENLI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process route has long steps, cumbersome operation and high cost, and is not suitable for industrial production

Method used

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  • Synthetic method of ethyl ethoxy acrylate
  • Synthetic method of ethyl ethoxy acrylate
  • Synthetic method of ethyl ethoxy acrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the autoclave, add 105.6g (1.2mol) of ethyl acetate, 68g (1mol) of sodium ethoxide, and 500ml of toluene, ventilate the kettle, feed CO to a pressure of 25atm, stir and react at 80°C for 2 hours, cool down, pressure to obtain a suspension of ethyl formyl acetate sodium salt, then add 46g (1mol) of ethanol, pass into 3g (0.08mol) of HCl gas, and then pass into CO 2 When the system pressure was 25 atm, the reaction was stirred at 110°C for 1.5 hours, cooled, reduced pressure, filtered, and the filtrate was distilled under reduced pressure to obtain 130 g of ethyl ethoxyacrylate (90°C, 25 mmHg), with a yield of 90.3%.

Embodiment 2

[0027] In the autoclave, add 88 g (1 mol) of ethyl acetate, 68 g (1 mol) of sodium ethoxide, and 500 ml of toluene, ventilate the autoclave, feed CO to a pressure of 10 atm, stir and react at 50 ° C for 5 hours, cool and depressurize, Prepare ethyl formyl acetate sodium salt suspension, then add 46 g (1 mol) of ethanol, feed 3 g (0.08 mol) of HCl gas, and then feed CO 2 When the system pressure was 20 atm, the reaction was stirred at 80°C for 4 hours, cooled, reduced pressure, and filtered, and the filtrate was distilled under reduced pressure to obtain 115.4 g of ethyl ethoxyacrylate (90°C, 25 mmHg), with a yield of 80.1%.

Embodiment 3

[0029] In the autoclave, add 140.8 g (1.6 mol) of ethyl acetate, 68 g (1 mol) of sodium ethoxide, and 500 ml of toluene, ventilate the autoclave, feed CO to a pressure of 50 atm, stir and react at 90° C. for 1 hour, cool down, pressure to obtain a suspension of ethyl formyl acetate sodium salt, then add 46g (1mol) of ethanol, pass into 3g (0.08mol) of HCl gas, and then pass into CO 2 When the system pressure was 25atm, the reaction was stirred at 110°C for 1.5 hours, cooled, reduced pressure, filtered, and the filtrate was distilled under reduced pressure to obtain 125.8 g of ethyl ethoxyacrylate (90°C, 25 mmHg), with a yield of 87.4%.

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Abstract

The invention discloses a synthetic method of ethyl ethoxy acrylate. The method comprises the following steps: reacting ethyl acetate and sodium ethoxide as raw materials in the presence of methylbenzene as a solvent under the condition that CO is introduced until the pressure is 10-50 atm, so as to prepare formyl ethyl acetate sodium salt suspension liquid; reacting the formyl ethyl acetate sodium salt suspension liquid with ethanol under the condition that HCl gas and CO2 are introduced until the pressure is 20-30 atm, so as to prepare a target product-ethyl ethoxy acrylate. According to the method, the reaction process is short, few byproducts are generated, and the yield is high; the used raw materials are cheap and easily available, the solvent-methylbenzene can be recycled, and the production cost is low; a catalytic amount of HCl gas is adopted, so that the use of a large amount of HCl is avoided; sodium salt is directly converted into the target product under the pressurized condition, so that the loss of the intermediate process is reduced and the yield is increased.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing ethyl ethoxy acrylate. technical background [0002] Ethoxyethyl acrylate, the chemical name is 3-ethoxyethyl acrylate, CAS No.: [1001-26-9], molecular formula: C 7 h 12 o 3 , molecular weight: 144.17, the structure is as follows: [0003] [0004] Ethoxyethyl acrylate is an important pharmaceutical and chemical intermediate with a wide range of uses. It can be used in the preparation of broad-spectrum antibacterial quinolones, in the production of acrylate adhesives, and as a key intermediate in the preparation of photosensitive materials. 3-Amino-3-ethoxyethyl acrylate, etc. There are few direct reports on the research and synthesis of ethyl ethoxy acrylate, and there are the following four synthetic methods in its literature (partially with reference to the synthetic method of methyl methoxy acrylate): [0005] 1. Addition of ethyl acrylate b...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C69/734
CPCC07C67/31C07C67/343C07C69/734C07C69/716
Inventor 吴政杰
Owner ZHEJIANG BENLI TECH CO LTD