Synthesis method of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone

A synthesis method, ethoxy technology, applied in the direction of condensation preparation of carbonyl compounds, organic chemistry, etc., can solve the problems of difficult recovery of by-product trifluoroacetyl, low boiling point of trifluoroacetyl chloride, high production cost, etc., to achieve convenient recovery and simple preparation , the effect of easy access

Pending Publication Date: 2022-07-29
SHIJIAZHUANG SAN TAI CHEM CO LTD
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Problems solved by technology

[0003] 4-Ethoxy-1,1,1-trifluoro-3-buten-2-one, as a trifluoromethyl-containing active compound with excellent performance, has a wide range of applications, and some of its downstream products have been commercialized , its demand is increasing every year with the promotion of applications, the original trifluoroacetyl chloride route as an electrolyte additive has high preparation costs, trifluoroacetyl chloride has a low boiling point, is difficult to store, and the by-product trifluoroacetyl chloride is difficult to recover , so we propose a synthetic method of 4-ethoxy-1,1,1-trifluoro-3-buten-2-one to solve the above problems

Method used

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  • Synthesis method of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone
  • Synthesis method of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone
  • Synthesis method of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone

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Embodiment 1

[0022] refer to Figure 1-3 , a synthetic method of 4-ethoxy-1,1,1-trifluoro-3-buten-2-one, comprising the following steps:

[0023] 1) In a reaction flask equipped with a fractionation column (connected to a condenser, and the receiving bottle is cooled with an ice-salt bath), add absolute ethanol, mercuric acetate, n-butyl vinyl ether, heat to reflux, and control the temperature at the top of the fractionation column At 36~37 ℃, distill out ethyl vinyl ether;

[0024] 2) get 0.6 moles of trifluoroacetic acid and 0.7 moles of dichloroacetic anhydride, react after adding the dehydration reactant to obtain trifluoroacetic anhydride, and the reaction equation is CF 3 COOH+(C l2 CHCO) 2O →(CF 3 CO) 2O +C l2 CHCOOH;

[0025] 3) 2-Propyn-1-ol and methyl chloroformate react under the action of dehydrating agent and catalyst at 20-40 ° C for 2 hours to obtain 4-ethoxy-1,1,1-trifluoro-3 -Buten-2-one.

[0026] The dehydration reactant in step 2) is one or more of toluene, xyle...

Embodiment 2

[0028] refer to Figure 1-3 , a synthetic method of 4-ethoxy-1,1,1-trifluoro-3-buten-2-one, comprising the following steps:

[0029] 1) In a reaction flask equipped with a fractionation column (connected to a condenser, and the receiving bottle is cooled with an ice-salt bath), add absolute ethanol, mercuric acetate, n-butyl vinyl ether, heat to reflux, and control the temperature at the top of the fractionation column At 36~37 ℃, distill out ethyl vinyl ether;

[0030] 2) get 0.4 moles of trifluoroacetic acid and 0.75 moles of dichloroacetic anhydride, add the dehydration reactant and react to obtain trifluoroacetic anhydride, and the reaction equation is CF 3 COOH+(C l2 CHCO) 2O →(CF 3 CO) 2O +C l2 CHCOOH;

[0031] 3) 2-Propyn-1-ol and methyl chloroformate react under the action of dehydrating agent and catalyst at 20-40 ° C for 2 hours to obtain 4-ethoxy-1,1,1-trifluoro-3 -Buten-2-one.

[0032] The dehydration reactant in step 2) is one or more of toluene, xylene, ...

Embodiment 3

[0034] refer to Figure 1-3 , a synthetic method of 4-ethoxy-1,1,1-trifluoro-3-buten-2-one, comprising the following steps:

[0035] 1) In a reaction flask equipped with a fractionation column (connected to a condenser, and the receiving bottle is cooled with an ice-salt bath), add absolute ethanol, mercuric acetate, n-butyl vinyl ether, heat to reflux, and control the temperature at the top of the fractionation column At 36~37 ℃, distill out ethyl vinyl ether;

[0036] 2) get 0.7 moles of trifluoroacetic acid and 0.9 moles of dichloroacetic anhydride, add the dehydration reactant and react to obtain trifluoroacetic anhydride, and the reaction equation is CF 3 COOH+(C l2 CHCO) 2O →(CF 3 CO) 2O +C l2 CHCOOH;

[0037] 3) 2-Propyn-1-ol and methyl chloroformate react under the action of dehydrating agent and catalyst at 20-40 ° C for 3 hours to obtain 4-ethoxy-1,1,1-trifluoro-3 -Buten-2-one.

[0038] The dehydration reactant in step 2) is one or more of toluene, xylene, c...

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Abstract

The invention discloses a synthesis method of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-one, which comprises the following steps: adding absolute ethyl alcohol, mercury acetate and n-butyl vinyl ether into a reaction flask which is provided with a fractionating column (connected with a condenser and cooled by an ice salt bath for the flask), heating and refluxing, controlling the temperature of the top of the fractionating column to 36-37 DEG C, evaporating out ethyl vinyl ether, and cooling to obtain the 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-one, namely the 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-one. The preparation method comprises the following steps: mixing ethyl vinyl ether and trifluoroacetic anhydride, adding a deacidification agent, and reacting at 50-110 DEG C for 2-4 hours to obtain the 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone. According to the method, trifluoroacetic anhydride is adopted to replace trifluoroacetyl chloride to serve as a reaction raw material, trifluoroacetic anhydride is easy to prepare and convenient to obtain, and large-batch production of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone is facilitated.

Description

technical field [0001] The invention relates to the field of battery electrolyte additives, in particular to a method for synthesizing 4-ethoxy-1,1,1-trifluoro-3-buten-2-one. Background technique [0002] Lithium battery electrolyte is the carrier of ion transport in the battery. Generally composed of lithium salts and organic solvents. The electrolyte plays the role of conducting ions between the positive and negative electrodes of the lithium battery, which is the guarantee for the lithium ion battery to obtain the advantages of high voltage and high specific energy. The electrolyte is generally prepared from high-purity organic solvents, electrolyte lithium salts, necessary additives and other raw materials under certain conditions and in a certain proportion. The main electrolytes used in lithium batteries are lithium perchlorate, lithium hexafluorophosphate, etc. However, batteries made of lithium perchlorate have poor low-temperature effects and are at risk of explos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/255C07C45/45
CPCC07C45/455C07C51/56C07C41/18C07C49/255C07C53/18C07C43/16
Inventor 田丽霞彭鹏鹏刘鹏张民张茜葛建民闫彩桥武利斌王军
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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