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Preparation method of alpha-fluoroacrylate

A technology of fluoroacrylate and fluoroacetate is applied in the field of preparation of α-fluoroacrylate, can solve the problems of low purity, low yield of α-fluoroacrylate, etc. high rate effect

Active Publication Date: 2012-10-17
厦门中坤化学有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0010] In order to solve the problems of low yield and low purity of α-fluoroacrylate obtained in the prior art, the present invention provides a preparation method of α-fluoroacrylate, and achieves the improvement of α-fluoroacrylate Esters Yield and Purity Objectives

Method used

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  • Preparation method of alpha-fluoroacrylate
  • Preparation method of alpha-fluoroacrylate
  • Preparation method of alpha-fluoroacrylate

Examples

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preparation example Construction

[0025] First, please refer to figure 1 , figure 1 It is a flow chart of the preparation method of a kind of α-fluoroacrylate of the present invention, from figure 1 It can be seen that the present invention comprises the following steps: Step 11: adding α-fluoroacetate to the mixed solution of oxalic acid diester and sodium alkoxide for reaction; the chemical reaction formula is:

[0026]

[0027] Step 12: Sodium salt is obtained after filtration, washing and drying

[0028] Step 13: The sodium salt is condensed with paraformaldehyde, and the α-fluoroacrylate is obtained after vacuum distillation. The chemical reaction formula is:

[0029]

[0030] R in the above two chemical reaction formulas is a C1-C8 alkyl group, and M is an alkaline earth metal ion such as sodium, potassium, lithium or the like. The alkyl group includes methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, n-pentyl, isopentyl, n-hexyl or isohexyl; alkaline earth metal ions include sodium, potass...

example 1

[0034] Example 1: Preparation of dimethyl sodium 2-fluoro-3-oxosuccinate

[0035] On the dried four-necked flask (500mL), add a condenser tube, a drying tube (anhydrous CaCl 2 ), thermometer, mechanical stirring, constant pressure dropping funnel. Sodium methoxide (56 g), freshly distilled dry methyl tert-butyl ether (dried over 4A molecular sieves) (400 mL), and dimethyl oxalate (118.09 g) were first added. The temperature of the external bath is controlled at about 30°C, and stirred for 30 minutes. Then methyl fluoroacetate (92.07 g) was added dropwise through a constant pressure dropping funnel to control the reaction at 30° C. (about 40 min). Stirring was continued at 20-30 °C until the reaction was complete (about 14 h). A large amount of light-colored finely divided powdery solid appeared in the reaction flask. The reaction liquid was filtered, and the filter cake was washed with anhydrous methyl tert-butyl ether (50 mL*3) until the washing liquid was colorless. Aft...

example 2

[0036] Example 2: Preparation of α-methyl fluoroacrylate

[0037] On the dried two-necked flask (500mL), add a 40mm glass sleeve, an exhaust joint, a thermometer, and a magnet. Add sodium dimethyl 2-fluoro-3-oxosuccinate (40 g) and dimethyl sulfoxide (300 mL) (dried over 4A molecular sieves), stir for 20 min, and then add paraformaldehyde (6 g). The temperature of the reaction solution was raised to 40° C., and the reaction was completed after about 1.5 h. Connect the vacuum distillation device, and carry out vacuum distillation operation [25mmHg / 60 ℃ (external bath temperature)]. Crude methyl α-fluoroacrylate was obtained. The crude product was washed with 60 mL of saturated saline solution. The upper organic phase was dried over anhydrous sodium sulfate. 19 g of methyl α-fluoroacrylate was obtained by filtration with a purity of >98%.

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Abstract

The invention provides a preparation method of alpha-fluoroacrylate. The preparation method comprises the following steps: reacting by adding alpha-fluoroacetate to a mixed solution of an oxalic acid diester and a sodium alkoxide; filtering, washing and drying to obtain a sodium salt; and condensing the sodium salt and a paraformaldehyde, and carrying out reduced pressure distillation to obtain the alpha-fluoroacrylate. The preparation method of the alpha-fluoroacrylate has the characteristics of simplicity, high yield, and no need of special equipment, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to the fields of chemical engineering and medicinal chemistry, in particular to a preparation method of α-fluoroacrylate. Background technique [0002] Various esters of α-fluoroacrylic acid are both raw materials required for chemical drugs and monomers for preparing plastic optical fibers. In terms of chemicals, as more and more products are compounds containing fluorine, their demand will also increase significantly. Optical fiber communication is the main force for information transmission, and fluorine-containing plastic optical fiber has the advantage of low light consumption. Therefore, as monomers for preparing them, their application prospects are quite huge. [0003] α-Fluoroacrylates can be synthesized by several methods: [0004] One is through the dehydration synthesis of 2-fluoropropionate (see literature Japanese Appl.60-78941; Japanese Appl.60-78942); chemical formula: [0005] The second is synthesized by de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/653C07C67/333
Inventor 李勇李晓强
Owner 厦门中坤化学有限公司
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