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Method for preparing 2-fluoroalkyl acrylate

A technology for fluoroacrylate and hydroxypropionate, which is applied in the field of preparing 2-fluoroacrylate, can solve the problems of complex process and harsh production conditions, and achieves the effects of low production process conditions, simple method and easy control.

Inactive Publication Date: 2011-10-12
YUANPING TONGLI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the shortcomings of complex process and harsh production conditions in the existing preparation method, and to provide a preparation method of 2-fluoroacrylate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 1 mol of 2-fluoro-3-hydroxypropionate methyl ester and 1 mol of acetic anhydride in a container and heat them together to 30°C, and react for 2 hours; cool down to 30°C, add 0.4g of hydroquinone, vacuumize, and keep the residual pressure at 250mmHg , Slowly raise the temperature, collect fractions at 120-160°C, and rectify the collected fractions to obtain 2-fluoroacrylate.

Embodiment 2

[0018] Put 1mol of ethyl 2-fluoro-3-hydroxypropionate and 1.5mol of acetic anhydride in a container and heat them together to 150°C for 8 hours; cool down to 30°C, add 0.4g of phenothiazine, vacuumize and keep the residual pressure at 250mmHg , Slowly raise the temperature, collect fractions at 120-160°C, and rectify the collected fractions to obtain 2-fluoroacrylate.

Embodiment 3

[0020] Put 1 mol of 2-fluoro-3-hydroxypropionate and 1.2 mol of acetic anhydride in a container, heat them together to 50°C, and react for 3 hours; cool down to 30°C, add 0.4g of phenothiazine, vacuumize, and keep the residual pressure at 250mmHg , Slowly raise the temperature, collect fractions at 120-160°C, and rectify the collected fractions to obtain 2-fluoroacrylate.

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PUM

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Abstract

The invention discloses a method for preparing 2-fluoroacrylate. The method comprises the following steps of: putting 2-fluoro-3-hydroxypropionate and acetic anhydride into a container, heating the 2-fluoro-3-hydroxypropionate and the acetic anhydride together to the temperature of between 30 and 150 DEG C, and reacting for 2 to 8 hours; and cooling to the temperature of 30 DEG C, adding a polymerization inhibitor, vacuumizing, keeping the excessive pressure at 250mmHg, slowly heating, collecting fractions of 120 to 160 DEG C, and rectifying the collected fractions to obtain the 2-fluoroacrylate. The method is simple and easy to control; requirements on production process condition are low, and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing 2-fluoroacrylate. Background technique [0002] Acrylate-based polymers are of great importance in modern technologies and processes. Among a series of such polymers, poly(2-fluoroacrylate) optical materials, which occupy a special position, are valued for their excellent transparency, impact resistance and heat resistance. However, due to the difficulty and high cost of the synthesis process of 2-fluoroacrylate, it can only be applied in special fields. [0003] The commonly used method of synthesizing 2-fluoroacrylate is to utilize Claisen ester condensation reaction to generate oxalyl fluoride acetyl ester, then add paraformaldehyde to obtain the crude product of 2-fluoroacrylate, then wash and dry, Distillation produces the final product. [0004] Li Li et al. introduced in the synthesis of α-methyl chloroacrylate and α-methyl fluoroacrylate [J] (Synthetic Chemistry, 2004 (06)): sequentially add so...

Claims

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Application Information

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IPC IPC(8): C07C69/653C07C67/327
Inventor 贺芬霞薄宪明张婧
Owner YUANPING TONGLI CHEM