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Synthetic method of (ethoxymethylene)-malononitrile

A technology of ethoxymethylene malononitrile and synthesis method, which is applied in chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc., can solve the problems of large amount of organic solvent, high reaction temperature, and yield of target product. Unsatisfactory efficiency and purity, etc., to achieve the effects of improving purity, lowering reaction temperature, and lowering cost

Active Publication Date: 2012-07-18
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defects of large amount of organic solvent, high reaction temperature, unsatisfactory target product yield and purity in the existing method for synthesizing ethoxymethylene malononitrile, the purpose of this invention is to provide a kind of ethoxymethylene malononitrile The synthetic method of methyl malononitrile

Method used

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  • Synthetic method of (ethoxymethylene)-malononitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Preparation of ethoxymethylene malononitrile:

[0027] In a 5000ml three-neck flask, install a thermometer, a condenser, and a mechanical stirrer, add 2600g of triethyl orthoformate, cool in an ice-water bath to about 20°C, and drop 1050g of malononitrile quickly and intermittently, without obvious heat release, drop after 30 minutes After the addition is complete, 10 g of anhydrous zinc chloride is added, heated in a water bath to 70° C., and stirred for 3 h. After the reaction, the ethanol generated by the reaction was distilled off, and a dark red solid was obtained after cooling. After crystallization in refrigeration, suction filtration was obtained to obtain the crude product of ethoxymethylene malononitrile (directly proceed to the next step of refining without drying).

[0028] 2) Refining of ethoxymethylene malononitrile:

[0029] Add the above crude product of ethoxymethylenemalononitrile into a 5000ml three-necked flask, install a thermometer, condenser, ...

Embodiment 2

[0031] 1) Preparation of ethoxymethylene malononitrile:

[0032] In a 5000ml three-necked bottle, install a thermometer, a condenser, and a mechanical stirrer. Add 2,600g of triethyl orthoformate, cool in an ice-water bath to about 20°C, add 1,100g of malononitrile intermittently and rapidly, without obvious exotherm, and complete the dropwise addition after 50 minutes, then add 10g of anhydrous zinc chloride, and heat in a water bath to 70 ° C, stirring the reaction for 2.5h. After the reaction, the ethanol generated by the reaction was distilled off, and a dark red solid was obtained after cooling. After crystallization in refrigeration, suction filtration was obtained to obtain the crude product of ethoxymethylene malononitrile (no drying, directly proceed to the next step of refining).

[0033] 2) Refining of ethoxymethylene malononitrile:

[0034] Add the above crude product of ethoxymethylenemalononitrile into a 5000ml three-necked flask, install a thermometer, condens...

Embodiment 3

[0036] 1) Preparation of ethoxymethylene malononitrile:

[0037] In a 5000ml three-necked bottle, install a thermometer, a condenser, and a mechanical stirrer. Add 2600g of triethyl orthoformate, cool in an ice-water bath to about 20°C, add 1160g of malononitrile intermittently and quickly, without obvious exotherm, and complete the dropwise addition after 40 minutes, then add 11g of anhydrous zinc chloride, and heat in a water bath to 70 ° C, stirring the reaction for 4h. After the reaction, the ethanol generated by the reaction was distilled off, and a dark red solid was obtained after cooling. After crystallization in refrigeration, suction filtration was obtained to obtain the crude product of ethoxymethylene malononitrile (no drying, directly proceed to the next step of refining).

[0038] 2) Refining of ethoxymethylene malononitrile:

[0039] Add the above crude product of ethoxymethylenemalononitrile into a 5000ml three-necked flask, install a thermometer, condenser, ...

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Abstract

The invention relates to a synthetic method of (ethoxymethylene)-malononitril, which includes the following steps: (1) dropwise adding malononitrile into triethyl orthoformate in ice bath cooling condition, and adding catalyst anhydrous zinc chloride after dropwise adding for reaction for 2-4 hours, and (2) steaming and removing ethanol after the reaction is finished, cooling for dissolving out solids, and filtering and collecting the solids to obtain the (ethoxymethylene)-malononitrile. The synthetic method is easy to operate, high in yield, low in cost, environment-friendly, high in product crystallization purity, stable in quality and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing a pharmaceutical intermediate ethoxymethylene malononitrile. Background technique [0002] Ethoxymethylenemalononitrile, as shown in formula I, Chinese alias: ethoxydicyanoethylene, ethoxymethylenemalononitrile, ethoxymethylenepropanediol, ethoxy Methylene malononitrile, ethoxymethenyl malononitrile. CAS registration number is 123-06-8, molecular formula C 6 h 6 N 2 O, molecular weight 122.1246. [0003] [0004] Formula I [0005] The appearance of ethoxymethylene malononitrile is white to off-white crystalline powder; insoluble in water, easily soluble in organic solvents such as ethanol, with a melting point of 65-67°C and a boiling point of 160°C (12mmHg). It can be used as an industrial and pharmaceutical intermediate, such as for the synthesis of milrinone. [0006] At present, the synthetic method of ethoxymethylene malononitrile is most...

Claims

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Application Information

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IPC IPC(8): C07C255/15C07C253/30
Inventor 张瑾汪洪湖张亚孙建华江立新韦亚锋陈昀
Owner BENGBU BBCA MEDICINE SCI DEV
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