Method for preparing 1,4-diethyleno dioxide ketone

A technology of dioxanone and ethylene glycol, applied in the direction of organic chemistry, etc., can solve the problems of purification and storage difficulties, production costs and safety hazards of target products, and lengthy steps, so as to eliminate difficulties and safety hazards and reduce separate preparation and purification, the effect of reducing the amount of solvent used

Inactive Publication Date: 2009-02-18
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for this synthetic route, these patents all adopt the step-by-step intermediate method of preparing the target product 1,4-dioxanone, and the steps are tedious, time-consuming and uneconomical.
Moreover, the purification and storage of some intermediates such as ethylene glycol salts are more difficult, which undoubtedly brings greater production costs and potential safety hazards to the synthesis of target products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of β-hydroxyethoxy sodium acetate and sodium chloride solid mixture

[0032] Add 825g of sodium hydroxide with a purity of 97% into a reactor with 4L of ethylene glycol and 1.5L of xylene under stirring, and react at 130-145°C for 4 hours under nitrogen protection, and collect the reaction product through a water separator. of water. After the reaction was completed, 925 g of chloroacetic acid was added with stirring, and reacted at 60-100° C. for 1 hour. After the reaction stopped, the xylene in the upper floor was separated, the solid-liquid mixture in the lower floor was distilled under reduced pressure, and most of the unreacted ethylene glycol was steamed to obtain a slurry mixture of β-hydroxyethoxy sodium acetate and sodium chloride, The mixture was washed with acetone and filtered to obtain a white solid mixture, which was dried to obtain 1950 g of a solid mixture of β-hydroxyethoxy sodium acetate and sodium chloride.

[0033] (2) Preparation o...

Embodiment 2

[0038] (1) Preparation of β-hydroxyethoxy sodium acetate and sodium chloride solid mixture

[0039]Add 460g of metallic sodium sand particles into a reactor with 5L of ethylene glycol under stirring, and react at 60-80°C under nitrogen protection. After the reaction, 950 g of chloroacetic acid was added with stirring, and reacted at 50-100° C. for 1 hour. After the reaction stopped, the solid-liquid mixture was evaporated under reduced pressure to remove most of the unreacted ethylene glycol to obtain a slurry mixture of β-hydroxyethoxy sodium acetate and sodium chloride, which was washed and filtered with acetone to obtain a white solid The mixture was dried to obtain 1997 g of a solid mixture of β-hydroxyethoxy sodium acetate and sodium chloride.

[0040] (2) Preparation of β-hydroxyethoxyacetic acid solution

[0041] Add 2L of absolute ethanol to the solid mixture of 1997g of β-hydroxyethoxy sodium acetate and sodium chloride, stir and mix well, then slowly add sulfuric a...

Embodiment 3

[0045] (1) Preparation of β-hydroxyethoxy calcium acetate and calcium chloride solid mixture

[0046] Add 525 g of calcium hydride particles with a content of 80% into a reactor with 5 L of ethylene glycol under stirring, and react at 60-100° C. under nitrogen protection. After the reaction, 950 g of chloroacetic acid was added with stirring, and reacted at 50-100° C. for 1 hour. After the reaction stopped, the solid-liquid mixture was evaporated under reduced pressure to remove most of the unreacted ethylene glycol to obtain a slurry mixture of β-hydroxyethoxy calcium acetate and calcium chloride, which was washed and filtered with acetone to obtain a white solid The mixture was dried to obtain 2020g of β-hydroxyethoxy calcium acetate and calcium chloride solid mixture.

[0047] (2) Preparation of β-hydroxyethoxyacetic acid solution

[0048] Add 2L of absolute ethanol to the above 2020g β-hydroxyethoxy calcium acetate and calcium chloride solid mixture, stir and mix well, t...

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PUM

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Abstract

The present invention relates to a preparation method of 1, 4-dioxane alkone, and provides a highly efficient, rapid method of preparing high-purity 1, 4-dioxane alkone, which has no heavy metal ions. In the method, glycol and chloroacetic acid or the chloroacetate are used as raw materials. The method is characterized in that the intermediate beta-hydroxyl ethoxy acetate of the 1, 4-dioxane alkone is synthesized in one step, and the 1, 4-dioxane alkone can be produced through acidification and ring formation. Because the beta-hydroxyl ethoxy acetate is synthesized in one step, the present invention has the advantages that the reaction time is greatly shortened, the reaction yield is improved, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing 1,4-dioxanone. technical background [0002] 1,4-dioxanone (p-dioxanone) (or 1,4-dioxanone, p-dioxanone) is an important organic chemical product with a wide range of uses. It is not only used in organic Synthesis, and it is also widely used in polymer synthesis. It is a monomer for synthesizing poly-1,4-dioxanone and poly-1,4-dioxanone copolymer. Its homopolymer or copolymer are very important biodegradable medical materials. These materials have been It is widely used in the production of medical devices, so the rapid, low-cost, and heavy metal-free synthesis of 1,4-dioxanone is particularly important. [0003] There are mainly two kinds of synthetic methods of 1,4-dioxanone: one is the catalytic oxidative dehydrogenation preparation method using diethylene glycol (diethylene glycol) (or claiming diethylene glycol) as raw material,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12
Inventor 陈栋梁李庆熊成东张盛蓝张志萍
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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