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Method for preparing 3,3-diethoxy ethyl acrylate

A technology of ethyl diethoxy acrylate and ethyl cyanoacetate, which is applied in the fields of medicine and sanitation and organic synthetic chemistry, can solve the problems of inaccurate pH value and practical operation difficulties, and achieve simplified operation process and reduced solvent anhydrous treatment and recovery, the effect of high yield

Inactive Publication Date: 2006-10-18
WUHAN UNIV
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  • Application Information

AI Technical Summary

Problems solved by technology

This method is inaccurate in adjusting the pH value of the reaction solution in the organic medium in the second step, and requires the regulator to be anhydrous, so the actual operation is more difficult

Method used

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  • Method for preparing 3,3-diethoxy ethyl acrylate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0015] At -20°C, add 9.8 grams (0.125 moles) of acetyl chloride to a three-necked flask containing 11.3 grams (0.1 moles) of ethyl cyanoacetate and 9.2 grams (0.2 moles) of absolute ethanol, and maintain the temperature After reacting for 72 hours, 23.0 grams (0.5 moles) of absolute ethanol were added to the reaction solution, reacted at 0°C for 7 days, reduced to 9mmHg, and collected fractions at 122 to 124°C to obtain 11.3 grams of colorless liquid. 60%.

Embodiment 2

[0017] At 25°C, add 7.8 grams (0.1 moles) of acetyl chloride to a three-necked flask containing 11.3 grams (0.1 moles) of ethyl cyanoacetate and 11.5 grams (0.25 moles) of absolute ethanol, and maintain this temperature for 24 After 1 hour, add 36.9 grams (0.8 moles) of dehydrated alcohol to this reaction solution again, react for 8 days at 25 DEG C, depressurize to 9mmHg, collect the cut of 122~124 DEG C, obtain 7.5 grams of colorless liquid, productive rate is 40 %.

Embodiment 3

[0019] At 30°C, add 6.5 grams (0.08 moles) of acetyl chloride to a three-necked flask containing 11.3 grams (0.1 moles) of ethyl cyanoacetate and 11.5 grams (0.25 moles) of absolute ethanol, and maintain this temperature for 36 After 1 hour, add 4.6 grams (0.1 moles) of absolute ethanol to this reaction solution again, react for 7 days at 45°C, reduce the pressure to 9mmHg, collect the cuts at 122~124°C, obtain 4.5 grams of colorless liquid, and the yield is 30 %.

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Abstract

The invention relates to a preparation method of 3,3-diethoxy ethyl acrylate, which comprises mixing ethyl cyanoacetate, absolute ethanol and acetyl chloride in a molar ratio of 1:2.0~3.0:0.8~1.25, and mixing them at -20 After reacting at ℃~45℃ for 10~72 hours, add 1~8 molar amount of ethyl cyanoacetate to the reaction liquid, and then react at -20℃~45℃ for 3~14 days to obtain 3,3- Ethyl Diethoxyacrylate. In the reaction process of the invention, other solvents and pH regulators for adjusting the pH value are not needed, the process is simple, the cost is low, the corrosion to equipment and the pollution to the environment are small, and the yield is high.

Description

technical field [0001] The invention discloses a new method for preparing 3,3-diethoxy ethyl acrylate. It belongs to the field of organic synthetic chemistry, and also belongs to the field of medicine and health. Background technique [0002] 3,3-Diethoxy ethyl acrylate has a very special structure, which is a kind of enal (ketone) acetal derivative, which has certain stability and activity, and can pass some classic organic synthesis reactions under milder conditions , to synthesize some special nitrogen-containing heterocyclic pharmaceutical and pesticide intermediates that are difficult to obtain by other synthetic methods. [0003] The main methods used to prepare 3,3-diethoxy ethyl acrylate at present abroad are: [0004] (1) The mixture of ethyl cyanoacetate, absolute ethanol and dry diethyl ether is fed with an appropriate amount of hydrogen chloride gas under cooling, and left to stand for 24 hours under cooling to obtain imine hydrochloride, which is then mixed wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/734C07C67/30
Inventor 邱国福胡先明姚二东徐雪松梁淑彩吴腊梅
Owner WUHAN UNIV
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