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Method for preparing 3-amino-4,4,4-trifluorocrotonate

A technology of ethyl trifluorocrotonate and ethyl trifluoroacetoacetate, which is applied in the field of preparation of ethyl 3-amino-4,4,4-trifluorocrotonate, can solve the problems of large equipment investment and achieve cost Economical, high yield, high content effect

Inactive Publication Date: 2016-10-05
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as the extractive distillation method is concerned, a higher concentration of acetic acid solution can be obtained by adding an extractant, but the equipment investment is large, and there are problems of extractant replenishment and recovery

Method used

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  • Method for preparing 3-amino-4,4,4-trifluorocrotonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The volume of the amination reaction kettle is 1000L, equipped with stirring, thermometer, metering tank and condenser. Add 368.0kg (2.0kmol) ethyl 4,4,4-trifluoroacetoacetate into the reaction kettle through the metering tank, and raise the temperature to 90°C after the addition is complete. Then throw in 323.4kg (4.2kmol) of ammonium acetate, and keep warm at 90°C for 3 hours after throwing in. Cool the temperature of the reaction solution to 30°C, stop stirring, and let stand for 30 minutes. The reaction solution is divided into two layers, the lower layer is an organic phase, the weight is 359.6kg, the content of the product 3-amino-4,4,4-trifluorocrotonate ethyl ester is 98.2%, and the yield is 96.5%; the upper layer is an aqueous phase, and the water The phase weight is 330.6kg, and the content of acetic acid in the water phase is 36.3%.

[0023] The resulting 359.6kg water phase was transferred to a 1000L neutralization reactor equipped with stirring, thermomet...

Embodiment 2

[0025] The volume of the amination reaction kettle is 1000L, equipped with stirring, thermometer, metering tank and condenser. Add 368.0kg (2.0kmol) ethyl 4,4,4-trifluoroacetoacetate into the reaction kettle through the metering tank, and raise the temperature to 100°C after the addition is complete. Then throw in 308.0kg (4.0kmol) of ammonium acetate, and keep warm at 80°C for 4 hours after throwing in. Cool the temperature of the reaction solution to 40°C, stop stirring, and let stand for 30 minutes. The reaction solution is divided into two layers, the lower layer is an organic phase, the weight is 357.6kg, the content of the product 3-amino-4,4,4-trifluorocrotonate ethyl ester is 97.7%, and the yield is 95.4%; the upper layer is an aqueous phase, water The phase weight is 317.5 kg, and the content of acetic acid in the aqueous phase is 38.5%.

[0026] The resulting 317.5kg water phase was transferred to a 1000L neutralization reactor equipped with stirring, thermometer, ...

Embodiment 3

[0028] The volume of the amination reaction kettle is 1000L, equipped with stirring, thermometer, metering tank and condenser. Add 414.0kg (2.25kmol) ethyl 4,4,4-trifluoroacetoacetate into the reaction kettle through the metering tank, and raise the temperature to 95°C after the addition is complete. Then drop into the ammonium acetate solid obtained in the embodiment 1 of 366.0kg (4.75kmol) and embodiment 2 (weight respectively accounts for 50%), after throwing, insulation 3 hours under 95 ℃. Cool the temperature of the reaction solution to 35°C, stop stirring, and let stand for 30 minutes. The reaction solution is divided into two layers, the lower layer is an organic phase, the weight is 403.5kg, the content of the product 3-amino-4,4,4-trifluorocrotonate ethyl ester is 98.2%, and the yield is 96.2%; the upper layer is an aqueous phase, and the water The weight of the phase is 375.4 kg, and the content of acetic acid in the water phase is 36.8%.

[0029] The resulting 403...

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Abstract

The invention discloses a method for preparing 3-amino-4,4,4-trifluorocrotonate with high raw material utilization rate. According to the invention, 4,4,4-trifluoroacetyl ethyl acetate and excessive ammonium acetate are subjected to an amination reaction to obtain a reaction solution, then the reaction solution is separated to an organic phase and an aqueous phase, ammoniacal liquor is added in the aqueous phase to obtain ammonium acetate, and finally ammonium acetate is cycled to continuous reaction.

Description

technical field [0001] The present invention relates to a preparation method of ethyl 3-amino-4,4,4-trifluorocrotonate, in particular to ethyl 3-amino-4,4,4-trifluorocrotonate with high raw material utilization rate method of preparation. Background technique [0002] Ethyl 3-amino-4,4,4-trifluorocrotonate is an active intermediate in the synthesis of pesticides, pharmaceuticals and other industrial chemicals, especially for the preparation of trifluoromethyl-substituted heterocyclic compounds, such as uracils derivatives, thiazole derivatives, oxazine derivatives and pyridine derivatives. [0003] For the preparation of ethyl 3-amino-4,4,4-trifluorocrotonate, it is generally prepared by amination reaction using ethyl 4,4,4-trifluoroacetoacetate and ammonium acetate as raw materials. This method can produce a large amount of by-products, that is, a mixture containing acetic acid and water. The prior art usually adopts four methods to separate acetic acid and water: ordinar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/30C07C227/06
Inventor 蒋强李华徐卫国陈伟
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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