Preparation method and refining method of ethoxymethylenemalononitrile

A technology of ethoxymethylene malononitrile and a refining method, which is applied in the preparation of carboxylic acid nitrile, the preparation of organic compounds, chemical instruments and methods, etc. Solvent recovery difficulties and other problems, to achieve the effect of solving the inconvenience of solvent recovery, improving the reaction speed and reaction yield, and facilitating solvent recovery and reuse

Inactive Publication Date: 2014-03-26
南京易亨制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Liu Qiming et al. (Liu Qiming, Su Yuyong, Chen Bangyin, Zhang Hanping. Synthesis and structural identification of phosphodiesterase inhibitor Milrinone [J]. Journal of Huazhong University of Science and Technology (Medical Science), 2005, 34(1): 74-75) published A kind of preparation method of ethoxymethylene malononitrile is proposed, and this method uses poisonous toluene in a large amount as solvent, and used catalyst zinc c

Method used

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  • Preparation method and refining method of ethoxymethylenemalononitrile
  • Preparation method and refining method of ethoxymethylenemalononitrile
  • Preparation method and refining method of ethoxymethylenemalononitrile

Examples

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Embodiment 1

[0024] Example 1 Preparation of ethoxymethylene malononitrile

[0025] In a 1L three-necked reaction flask, add 56g (0.848mol) malononitrile, 150g (1.013mol) triethyl orthoformate and 3g anhydrous lithium chloride, turn on the stirring, heat up to 90℃, reflux and keep for 3h, usually The ethanol produced by the reaction was removed by pressure distillation, the remaining liquid was frozen and crystallized (-5~0℃), filtered with suction, the solid was collected, and dried to obtain 79g of crude ethoxymethylenemalononitrile, with a yield of 76.5% About, the melting point is 64-67℃.

Embodiment 2

[0026] Example 2 Preparation of ethoxymethylene malononitrile

[0027] In a 5L three-necked reaction flask, add 1Kg (15.15mol) malononitrile, 3.2Kg (21.59mol) triethyl orthoformate and 60g anhydrous lithium chloride, stir, heat up to 85℃, reflux and keep for 3h, usually The ethanol produced by the reaction was removed by pressure distillation, the remaining liquid was frozen and crystallized (-5~0℃), solid-liquid separation, the solid was collected, and dried to obtain the crude ethoxymethylene malononitrile dry product 1.35Kg, the yield About 73.2%, the melting point is 65-67°C.

Embodiment 3

[0028] Example 3 Preparation of ethoxymethylene malononitrile

[0029] In a 50L reactor, add 7Kg (105.96mol) of malononitrile, 20Kg (134.95mol) of triethyl orthoformate and 375g of anhydrous LiCl, stir, heat up to 85°C, reflux for 3h, and then distill to remove The ethanol produced by the reaction, the remaining liquid is subjected to freezing crystallization (-5~0℃), solid-liquid separation, solid-liquid separation, solid-liquid separation, solid-liquid collection, and drying to obtain crude ethoxymethylenemalononitrile dry product 10.8Kg, yield 83.5% about. Melting point 64-67°C.

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Abstract

The invention relates to a preparation method and a refining method of ethoxymethylenemalononitrile. The preparation method comprises the steps as follows: putting malononitrile, triethyl orthoformate and anhydrous lithium chloride in a reaction vessel, stirring the mixture, heating the mixture to the temperature of 78-85 DEG C, after complete reaction, removing ethanol produced in the reaction through distillation, cooling and crystallizing the residual liquid after distillation, and collecting and drying solids to obtain the ethoxymethylenemalononitrile. According to the preparation method, a catalyst is changed into the anhydrous lithium chloride, the full contact of the catalyst with reaction substances is promoted, the ethanol produced in the reaction is directly used as a reaction solvent, and a synthetic reaction is performed at an ethanol backflow temperature, so that the catalytic efficiency, the reaction speed and the reaction efficiency are improved remarkably, the use of a large number of toxic solvents (methylbenzene) is avoided, the environmental protection is facilitated, the reaction operation is simplified, the problem of inconvenience in solvent recovery is solved, the manufacturing cost is reduced remarkably (the cost is reduced by about 40%), and the preparation method is applicable to the industrial production.

Description

Technical field [0001] The invention relates to the technical field of compound preparation, in particular to a preparation method and a refining method of ethoxymethylene malononitrile. Background technique [0002] Ethoxymethylenemalononitrile (Ethoxymethylenemalononitrile, structure shown in formula 1) is also known as ethoxydicyanoethylene, ethoxymethylenemalononitrile, ethoxymethylenemalononitrile, ethoxy Methylalkenylmalononitrile, CAS registration number is 123-06-8, molecular formula is C 6 H 6 N 2 O, the molecular weight is 122.1246. [0003] [0004] Ethoxymethylene malononitrile is white to off-white crystalline powder, insoluble in water, soluble in organic solvents such as methanol, ethanol, melting point 65℃-67℃, boiling point 160℃ (12mmHg), commonly used in the preparation of industrial chemicals , Intermediates of pharmaceutical chemicals, such as intermediates for the preparation of milrinone. [0005] At present, the preparation method of ethoxymethylene malononit...

Claims

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Application Information

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IPC IPC(8): C07C255/15C07C253/30C07C253/34
Inventor 冯维兵张丽红潘朝晖严晓星庄炜封思阳
Owner 南京易亨制药有限公司
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