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Technology of synthesizing 2,3-dicyano ethyl propionate

A technology of ethyl dicyanopropionate and ethyl cyanoacetate, which is applied in the preparation of cyanide reaction, organic chemistry, etc., can solve the problem of large loss of ethanol solvent, low yield of ethyl 3-cyanopropionate, and high price. Advanced problems, to achieve the effect of reducing production costs, good product quality, and small dielectric loss

Inactive Publication Date: 2006-06-14
栾忠岳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. The yield of finished product ethyl 2,3-dicyanopropionate is low, the highest can only reach 78%;
[0005] 2. The quality of the produced ethyl 2,3-dicyanopropionate product is not ideal, and the content of ethyl 2,3-dicyanopropionate can only be 93-95%
[0006] 3. The raw material potassium cyanide is highly toxic and expensive
[0007] 4. The loss of the ethanol solvent used is relatively large, and the recovery rate of ethanol is less than 65%.

Method used

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  • Technology of synthesizing 2,3-dicyano ethyl propionate
  • Technology of synthesizing 2,3-dicyano ethyl propionate
  • Technology of synthesizing 2,3-dicyano ethyl propionate

Examples

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Embodiment 1

[0023] Embodiment 1: The following is an industrial production embodiment.

[0024] see figure 1 , figure 2 , image 3 and Figure 4 .

[0025] 1. Use the following raw materials and reaction medium:

[0026] Ethyl cyanoacetate raw material content: >99%.

[0027] Raw material content of paraformaldehyde: 93-95%.

[0028] The sodium cyanide raw material of solid matter is an industrial superior product.

[0029] The reaction medium is dimethyl sulfoxide, its content: ≥98%.

[0030] 2. Take 3 barrels of medium dimethyl sulfoxide liquid, about 600-650 kg and 95 kg of raw material ethyl cyanoacetate liquid, from figure 1 The reaction kettle R1 can be seen, open the vacuum valve (7) in the 1500-liter glass-lined reaction kettle R1, and connect the vacuum pipeline through the vacuum direction C to the vacuum pump, so that the reaction kettle R1 is under negative pressure, and the liquid material is discharged from the suction port valve (4) Pump into the reaction kettle R...

Embodiment 2

[0059] 1, the raw material that adopts and reaction medium are identical with embodiment 1.

[0060] 2. Inhale 6 barrels of medium dimethyl sulfoxide (about 1200 kg to 1300 kg) and 190 kg of raw material ethyl cyanoacetate from the liquid material suction valve (4) of the reactor R1 into the reactor, and turn on the mixer (6), And open the cooling brine valve (3) so that the brine enters the kettle inner jacket (10) from the inlet direction B to cool down through the cooling brine outlet (9), and the cooling brine flows back to the brine storage tank in the direction D.

[0061] 3. Add 100 kilograms of solid raw material sodium cyanide and 50 kilograms of paraformaldehyde into the kettle from the manhole (8) of the reactor R1.

[0062] 4. Close the manhole cover of the manhole (8) of the reactor R1, make the temperature of the material in the reactor R1 be 10° C. to 30° C. by the above-mentioned cooling brine, and react under normal pressure for about 20 hours.

[0063] 5. Af...

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Abstract

The present invention relates to a process for synthesizing ethyl-2,3-dicyano-propionate which is used for produce pesticide intermediate. The basic method of said process includes the following steps: using the raw materials of ethyl cyanoacetate, paraformaldehyde and sodium cyanide to synthesize ethyl-2,3-dicyano-propionate in the medium dimethyl sulfoxide; after the ethyl-2,3-dicyano-propionate is synthesized, using solvent dichloromethane to extract the synthesized ethyl-2,3-dicyano-propionate from medium dimethyl sulfoxide, reduced pressure desolventizing to obtain crude product, then rectifying said crude product so as to obtain the refined product ethyl-2,3-cyano-propionate. Said invention also provides the concrete requirements of the above-mentioned every step. The purity of the obtained product is greater than 98%.

Description

Technical field: [0001] A process for synthesizing ethyl 2,3-dicyanopropionate of the present invention relates to the production of pesticide intermediates, ethyl 2,3-dicyanopropionate is a new type of high-efficiency and low-residue insecticide fipronil (Also known as fipronil) one of the main intermediates. Background technique: [0002] In the past, the process of producing 1,2-dicyanopropionate ethyl was to use ethanol as the medium solvent, that is, the raw materials ethyl cyanoacetate, potassium cyanide and paraformaldehyde were synthesized in the ethanol medium to produce 2,3-dicyanopropionate Ethyl cyanopropionate. [0003] There is following shortcoming in the production technology of above-mentioned previous 2,3-dicyanopropionate ethyl ester: [0004] 1. The yield of finished product ethyl 2,3-dicyanopropionate is low, the highest can only reach 78%; [0005] 2. The quality of the produced ethyl 2,3-dicyanopropionate is not ideal, and the content of ethyl 2,3-d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/16C07C255/04
Inventor 栾忠岳
Owner 栾忠岳
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