Synthetic method of difluoroethanol acetate

A technique for the synthesis of difluoroethanol acetate, which is applied in chemical instruments and methods, preparation of carboxylic acid salts, preparation of carboxylic acid halides, etc., can solve the problem of high storage conditions of acetyl chloride, affecting product yield and purity, Easy to decompose and other problems, to achieve the effect of reducing the difficulty of the reaction, improving the yield and purity, and simple raw materials

Pending Publication Date: 2022-05-17
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation of difluoroethanol acetate mainly adopts the reaction of acetyl chloride and difluoroethanol, but the storage conditions of acetyl chloride itself are relatively high, and it is easy to decompose, which affects the yield and purity of the final product.

Method used

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  • Synthetic method of difluoroethanol acetate
  • Synthetic method of difluoroethanol acetate
  • Synthetic method of difluoroethanol acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0022] The synthetic method of difluoroethanol acetate, its synthetic steps are as follows:

[0023] Take 18g (0.3mol) of glacial acetic acid and cool it down to 0°C, and slowly add 15.3g (0.1mol) of phosphorus oxychloride dropwise. After the reaction, let stand to separate layers, take the upper layer, and obtain the crude product of acetyl chloride, which can be directly subjected to the acylation reaction without post-treatment and drying;

[0024] Dissolve the obtained acetyl chloride in 30mL of dichloromethane, lower the temperature to 0°C again, slowly add 20g of triethylamine dropwise, maintain 0°C and slowly add 24.6g (0.3mol) of difluoroethanol dropwise (the duration of the dropwise addition is 1h), dropwise After completion, react for 1.5h, then slowly add 81g of triethylamine dropwise (the total amount of triethylamine added twice is 101g, i.e. 1mol), after the addition of triethylamine is completed, react for 1h, heat up to 10°C and continue the reaction to Acetyl...

Embodiment 2

[0027] The synthetic method of difluoroethanol acetate, its synthetic steps are as follows:

[0028] Take 18.6g (0.31mol) of glacial acetic acid and cool it down to 0°C, and slowly add 15.3g (0.1mol) of phosphorus oxychloride dropwise. After the acetylation reaction, let stand to separate layers, take the upper layer, and obtain the crude product of acetyl chloride, which can be directly carried out the acylation reaction without post-treatment and drying;

[0029] Dissolve the obtained acetyl chloride in 35mL of dichloromethane, lower the temperature to 5°C again, slowly add 20g of pyridine dropwise, and slowly add 23.78g (0.29mol) of difluoroethanol dropwise at 5°C (the duration of dropping is 40min). , react for 1 hour, then slowly add 67.01g of pyridine dropwise (the total amount of pyridine added twice is 87.01g, that is, 1.1mol). 50 mL of water was added for washing, and the phases were separated. The obtained organic phase was dried over anhydrous magnesium sulfate and...

Embodiment 3

[0031] The synthetic method of difluoroethanol acetate, its synthetic steps are as follows:

[0032] Take 18.3g (0.305mol) of glacial acetic acid and cool it down to 1°C, and slowly add 15.3g (0.1mol) of phosphorus oxychloride dropwise. After the acetylation reaction, let stand to separate layers, take the upper layer, and obtain the crude product of acetyl chloride, which can be directly carried out the acylation reaction without post-treatment and drying;

[0033] Dissolve the obtained acetyl chloride in 28mL of dichloromethane, lower the temperature to 1°C again, slowly add 15g of triethylamine dropwise, maintain 1°C and slowly add 24.19g (0.295mol) of difluoroethanol dropwise (the duration of dropping is 50min), dropwise After completion, react for 1.8h, then slowly add 75.9g of triethylamine dropwise (the total amount of triethylamine added twice is 90.9g, i.e. 0.9mol), after the addition of triethylamine is completed, react for 1.5h, and heat up to 11 Continue the react...

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Abstract

The invention discloses a synthesis method of difluoroethanol acetate, and relates to the technical field of battery electrolyte additives, the synthesis method comprises the following steps: taking glacial acetic acid, cooling to below 5 DEG C, slowly dropwise adding phosphorus oxychloride, carrying out acylating chlorination reaction, standing for layering, directly dissolving an obtained acetyl chloride crude product in dichloromethane, cooling to below 5 DEG C again, slowly dropwise adding difluoroethanol, and carrying out acylating chlorination reaction to obtain the difluoroethanol acetate. And after dropwise adding, carrying out acylation reaction under the catalytic action of an acid capturing agent to obtain the difluoroethanol acetate. According to the method, acetic acid is taken as a raw material, difluoroethanol acetate is synthesized through a one-pot method, post-treatment is not needed in the process, and the reaction difficulty is reduced; the adopted raw materials are simple and easy to obtain, and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of battery electrolyte additives, in particular to a synthesis method of difluoroethanol acetate. Background technique [0002] Lithium battery is a new type of green secondary battery successfully developed in the 1990s. Because of its advantages such as high energy density, high working voltage and long cycle life, it has become the most popular secondary battery at present. With the rapid development of lithium batteries, many problems have emerged, among which safety and stability are one of the most urgent problems to be solved. [0003] Difluoroethanol acetate is a new additive used in lithium battery electrolyte, which can improve the safety and stability of the battery and reduce the loss in the process of electric energy conversion. [0004] At present, the preparation of difluoroethanol acetate mainly uses acetyl chloride and difluoroethanol to react, but the storage conditions of acetyl chloride ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/14C07C69/14
CPCC07C67/14C07C51/60C07C69/14C07C53/40Y02E60/10
Inventor 张民彭鹏鹏郝俊侯荣雪王军
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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