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Synthetic method of ethyl 4,4,4-trifluoroacetoacetate

A technology of ethyl trifluoroacetoacetate and its synthesis method, which is applied in the field of synthesis of ethyl 4,4,4-trifluoroacetoacetate, and can solve the problems of multiple side reactions and potential safety hazards in production

Active Publication Date: 2021-07-06
山东京博生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at problems such as many side reactions and production safety hazards in the method for synthesizing ethyl 4,4,4-trifluoroacetoacetate in the prior art, the present invention provides a method for synthesizing ethyl 4,4,4-trifluoroacetoacetate Synthetic approach to address the above problems

Method used

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  • Synthetic method of ethyl 4,4,4-trifluoroacetoacetate
  • Synthetic method of ethyl 4,4,4-trifluoroacetoacetate

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Experimental program
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Effect test

Embodiment 1

[0031] (1) Weigh 114.3g (1.0mol) of trifluoroacetone and 228.6g of toluene and stir them evenly in a mixing bottle as liquid A; 110.2g (1.0mol) of ethyl chloroformate (content 98.5%) is used as liquid B;

[0032] (2) Set the temperature of the pipeline reactor to 50°C, the pressure to 0.5MPa, the pump A to set the flow rate at 8ml / min, and the pump B to set the flow rate to 2ml / min. After reaching the set temperature, open the tail gas exhaust valve and the hydrogen chloride gas inlet valve. Introduce hydrogen chloride gas; turn on pump A to feed the mixture of trifluoroacetone and toluene, and turn on pump B to feed ethyl chloroformate;

[0033] (3) after 20min, take a sample and detect 0.49% of the residual ethyl chloroformate in the reaction liquid at the outlet of the reactor, and the reaction is qualified;

[0034] (4) After the reaction is over, the reaction solution undergoes an atmospheric rectification to recover toluene and a small amount of residual raw materials, a...

Embodiment 2

[0036] (1) Weigh 125.7g (1.1mol) of trifluoroacetone and 377.1g of cyclohexane and stir them evenly in a mixing bottle as liquid A; 110.2g (content 98.5%) (1.0mol) of ethyl chloroformate as liquid B;

[0037] (2) Set the temperature of the pipeline reactor to 70°C, the pressure to 0.6MPa, the flow rate of pump A to 9.5ml / min, and the flow rate of pump B to 1.5ml / min. After reaching the set temperature, open the tail gas exhaust valve and hydrogen chloride gas intake Valve, feed hydrogen chloride gas; open pump A to enter the mixed solution of trifluoroacetone and cyclohexane, open pump B to enter ethyl chloroformate;

[0038] (3) After 20min, take a sample and detect 0.45% of the residual ethyl chloroformate in the reaction liquid at the outlet of the reactor, and the reaction is qualified;

[0039] (4) After the reaction is over, the reaction solution undergoes a rectification at atmospheric pressure to recover cyclohexane and a small amount of residual raw materials, and the...

Embodiment 3

[0041] (1) Weigh 125.7g (1.1mol) of trifluoroacetone and 377.1g of cyclohexane and stir them evenly in a mixing bottle as liquid A; 110.2g (1.0mol) of ethyl chloroformate (content 98.5%) is used as liquid B;

[0042] (2) Set the temperature of the pipeline reactor to 80°C, the pressure to 0.7MPa, set the flow rate of pump A to 9.5ml / min, and the flow rate of pump B to 1.5ml / min, and open the tail gas exhaust valve and hydrogen chloride gas intake after reaching the set temperature Valve, feed hydrogen chloride gas; open pump A to enter the mixed solution of trifluoroacetone and cyclohexane, open pump B to enter ethyl chloroformate;

[0043] (3) After 20min, take a sample and detect 0.2% of the residual ethyl chloroformate in the reaction liquid at the outlet of the reactor, and the reaction is qualified;

[0044] (4) After the reaction is over, the reaction solution undergoes a rectification at atmospheric pressure to recover cyclohexane and a small amount of residual raw mate...

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Abstract

The invention relates to a synthetic method of ethyl 4,4,4-trifluoroacetoacetate, belonging to the field of chemical synthesis. According to the invention, trifluoroacetone and ethyl chloroformate are used as raw materials, hydrogen chloride is used as a catalyst, and a reaction is carried out in a pipeline reactor. The invention provides the novel method for synthesizing the ethyl 4,4,4-trifluoroacetoacetate; and the ethyl chloroformate with higher reaction activity is adopted and the reaction is catalyzed by hydrogen chloride, so reaction time is shortened, the self-condensation reaction of the ethyl 4,4,4-trifluoroacetoacetate in strong acid and strong alkali systems is avoided, and reaction yield and product purity are improved.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and specifically provides a method for synthesizing ethyl 4,4,4-trifluoroacetoacetate. Background technique [0002] 4,4,4-Ethyl trifluoroacetoacetate is an important intermediate in the synthesis of pesticides and medicines, and can be used for the preparation of flonicamid, thiafluzamide, pyrimaben, thiazox, etc. Currently, 4,4, There are two main methods for ethyl 4-trifluoroacetoacetate: [0003] (1) The Claisen condensation method is prepared by using ethyl trifluoroacetate and ethyl acetate as raw materials and reacting them in an ethanol solution of sodium ethoxide. This method is the most commonly used method, but in order to prevent the raw materials ethyl trifluoroacetate and ethyl acetate from undergoing transesterification or hydrolysis to generate impurities, the alkali selected is ethanol solution of sodium ethoxide, and the intermediate state 3-ethoxy Ethyl-3-hydroxyl-4,4,4-trif...

Claims

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Application Information

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IPC IPC(8): C07C69/716C07C67/313C07C67/54
CPCC07C67/313C07C67/54C07C69/716
Inventor 张思思张永军于连友王光金景伟伟侯继敏李冰洁
Owner 山东京博生物科技有限公司
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