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A kind of synthetic method of 4,4,4-trifluoroethyl acetoacetate

A technology of ethyl trifluoroacetoacetate and a synthesis method, which is applied in the field of synthesis of ethyl 4,4,4-trifluoroacetoacetate, can solve the problems of side reactions and many hidden dangers in production, and achieves the effect of improving mass transfer and heat transfer. , High environmental benefits, avoid the accumulation of by-products

Active Publication Date: 2022-07-15
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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  • A kind of synthetic method of 4,4,4-trifluoroethyl acetoacetate
  • A kind of synthetic method of 4,4,4-trifluoroethyl acetoacetate
  • A kind of synthetic method of 4,4,4-trifluoroethyl acetoacetate

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Experimental program
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Effect test

Embodiment 1

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

[0032] (2) the temperature of the pipeline reactor is set to 50°C, the pressure is 0.5MPa, the flow rate of the pump A is set to 8ml / min, the flow rate of the pump B is set to 2ml / min, and the exhaust gas exhaust valve and the hydrogen chloride gas inlet valve are opened after reaching the set temperature, Introduce hydrogen chloride gas; open pump A to enter the mixed solution of trifluoroacetone and toluene, open pump B to enter ethyl chloroformate;

[0033] (3) 0.49% residual ethyl chloroformate of the reaction solution at the outlet of the reactor was detected by sampling after 20 min, and the reaction was qualified;

[0034] (4) after the reaction finishes, the reaction solution recovers toluene and a small amount of residual raw materials through a norm...

Embodiment 2

[0036] (1) 125.7 g (1.1 mol) of trifluoroacetone and 377.1 g of cyclohexane were weighed and stirred in a mixing bottle to serve as solution A; 110.2 g of ethyl chloroformate (content 98.5%) (1.0 mol) was used as solution B;

[0037] (2) The temperature of the pipeline reactor is set to 70°C, the pressure is 0.6MPa, the flow rate of the pump A is set to 9.5ml / min, and the flow rate of the pump B is set to 1.5ml / min. After reaching the set temperature, open the exhaust exhaust valve and the hydrogen chloride gas inlet. 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) 0.45% residual ethyl chloroformate of the reaction solution at the outlet of the reactor was detected by sampling after 20 minutes, and the reaction was qualified;

[0039] (4) after the reaction finishes, the reaction solution recovers cyclohexane and a small amount of residual raw materials throug...

Embodiment 3

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

[0042] (2) The temperature of the pipeline reactor is set to 80°C, the pressure is 0.7MPa, the flow rate of pump A is set to 9.5ml / min, and the flow rate of pump B is set to 1.5ml / min. After reaching the set temperature, open the exhaust gas exhaust valve and the hydrogen chloride gas inlet. 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) 0.2% residual 0.2% of ethyl chloroformate in the reaction solution at the outlet of the reactor is detected by sampling after 20 minutes, and the reaction is qualified;

[0044] (4) after the reaction finishes, the reaction solution recovers cyclohexane and a small amount of residual raw materials throug...

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Abstract

The invention relates to a method for synthesizing ethyl 4,4,4-trifluoroacetoacetate, and belongs to the field of chemical synthesis. The invention adopts trifluoroacetone and ethyl chloroformate as raw materials, and uses hydrogen chloride as a catalyst to carry out the reaction in a pipeline reactor. The invention provides a new method for synthesizing ethyl 4,4,4-trifluoroacetoacetate, which adopts ethyl chloroformate with higher reactivity, and uses hydrogen chloride to catalyze the reaction, shortens the reaction time, and avoids 4,4,4 ‑The self-condensation reaction of ethyl trifluoroacetoacetate in the strong acid and strong base system improves the yield of the reaction and the purity of the product.

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] Ethyl 4,4,4-trifluoroacetoacetate is an important intermediate for the synthesis of pesticides and medicines. It can be used to prepare flonicamid, thiflufenamide, pyrimethoxine, dichlorpyrifosin, etc. Currently, 4,4, The main methods of ethyl 4-trifluoroacetoacetate are as follows: [0003] (1) Claisen condensation method, using ethyl trifluoroacetate and ethyl acetate as raw materials, and reacting in an ethanolic solution of sodium ethoxide. This method is the most commonly used method, but in order to prevent the raw material ethyl trifluoroacetate and ethyl acetate from being transesterified or hydrolyzed to generate impurities, the selected alkali is the ethanolic solution of sodium ethoxide, and the intermediate state 3-ethoxylate generated by the reaction Ethyl-3-hydroxy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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