Preparation method of vinyl ether compound

Abstract

The invention discloses a preparation method of a vinyl ether compound. The vinyl ether compound is benzyloxy vinyl ether or triethyleneglycol divinyl ether. The preparation method is characterized by comprising the following steps: 1, preparing a catalyst [Ir(COD)Cl]2, wherein the catalyst [Ir(COD)Cl]2 is prepared by dissolving iridous chloride and 1,5-cyclooctadiene in water and alcohol and performing reflux reaction under waterless and oxygen-free conditions; 2, dissolving the catalyst [Ir(COD)Cl]2 and raw materials such as alcohol, vinyl acetate and sodium carbonate, and performing reflux reaction under a waterless and oxygen-free atmosphere; and 3, after the reaction is finished, washing with water, performing reduced pressure distillation, and performing column chromatography to obtain the product. The preparation method effectively solves the problems of high catalyst cost, high reaction temperature, complicated operation, high solvent toxicity and the like in the prior art, thereby providing a green preparation method of a vinyl ether compound, which has the advantages of high yield and simple operation steps.

Description

1. Technical field [0001] The invention belongs to the field of organic compound synthesis, and in particular relates to a preparation method of vinyl ether compounds. 2. Background technology [0002] Vinyl ether monomers can be used as reactive diluents in systems such as epoxy resins, acrylic resins, and unsaturated polyesters, and have broad application space in the fields of electronic materials, inks, printing, and coatings. The country started relatively late in this aspect, and the monomer production has not yet been industrialized, and the commercially available products are all imported from abroad, so it is of great significance to rapidly develop my country's vinyl ether series products. [0003] Due to the particularity of the preparation methods of vinyl ether compounds, since the 1930s, most of the preparation methods of vinyl ether compounds have applied for patents for protection, including BASF, DuPont, Standard Oil, General Electric and other large compani...

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Problems solved by technology

[0008] The product can be obtained in one step in this reaction, but problems such as high-pressure and high-temperature equipment, the explosion hazard of acetylene gas, and low yield have not been resolved;

However, the reaction conditions are harsh and unfavorable for industrialization

[0016] At present, the alcohol exchange method is more researched, using alcohol as raw material, under the catalysis of [Ir(COD)Cl]2 and alkali, in the atmosphere of nitrogen protection, the vinyl group of vinyl acetate is transferred to the alcohol. The yield is high, but the catalyst is expensive, and there are problems such as high temperature reaction, complicated operation, and high solvent toxicity.

[0017] Literature (Yoshio Okimoto.Development of a Highly Efficient Catalytic Method for Synthesis of Vinyl Ether.J.Am.Chem.Soc.2002,124,1590-1591) uses alcohol exchange method, using alcohol as raw material, in [Ir(COD)Cl] 2 Under the catalysis of sodium acetate, the vinyl group of vinyl acetate is transferred to alcohol, but sodium acetate is easy to absorb water, weathered and flammable, and there is danger. In addition, the catalyst [Ir(COD)Cl] in this document 2 The preparation requires high-temperature reflux, the operation is complicated, and toluene is used as a solvent, which is highly toxic and does not meet the purpose of green chemistry

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