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Synthetic method of benzenesulfonate derivative

A technology of benzenesulfonate ester and synthesis method, which is applied in the field of synthesis of benzenesulfonate derivatives, can solve the problems of complex synthesis method, battery performance degradation, damage, etc., and achieve simple synthesis method and enhanced high and low temperature stability Effect

Inactive Publication Date: 2018-03-27
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A lithium battery includes a positive electrode, a negative electrode, an electrolyte, and a separator. However, during the charging and discharging process, the battery will release heat, resulting in a decrease in battery performance.
During the charging and discharging process, the battery will release heat, which will reduce the performance of the battery. When the existing electrolyte additives encounter high temperature conditions during use, the performance of the battery is poor and the damage is serious. , will cause serious capacity reduction. In order to overcome the above shortcomings, we are committed to researching an electrolyte additive, which can effectively improve the performance of the battery under high temperature conditions.
[0003] Benzenesulfonate derivatives are important organic synthesis intermediates and are widely used. We have found through research that they can be applied to battery electrolytes, but their synthesis methods are complicated. At present, there is no method to prepare them into batteries that meet the requirements of battery electrolytes. Require

Method used

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  • Synthetic method of benzenesulfonate derivative
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  • Synthetic method of benzenesulfonate derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 1.0mol of phenol and 500ml of dichloromethane into the reaction flask respectively, add triethylamine under stirring, then cool down to below 15°C, start to add 1.1mol of benzenesulfonyl chloride dropwise, return to room temperature and continue stirring for 1h, then raise the temperature The reaction was continued at reflux for 2 hours. After the reaction was completed by gas phase detection, it was ice-thawed, separated, dried and concentrated to obtain the crude product and then recrystallized to obtain 222.3 g of the pure product. The calculated yield of the product was 95%. The detection purity is 99.93%, the moisture content is 30ppm, the acid value is 34ppm, and the measured density is 1.277g / cm 3 , with a boiling point of 375.4°C and 760mmHg, and its 1H NMR spectrum is as follows figure 1 As shown, the 13CNMR spectrum is as figure 2 shown.

[0021] The synthetic route is:

[0022]

Embodiment 2

[0024] Add 1.0mol of allyl alcohol and 500ml of dichloromethane into the reaction flask respectively, add pyridine under stirring, then cool down to below 15°C, start to add 2.1mol of benzenesulfonyl chloride dropwise, return to room temperature and continue stirring for 1h, and then raise the temperature to The reaction was continued under reflux for 2 hours. After the reaction was completed by gas phase detection, it was ice-thawed, separated into layers, dried and concentrated to obtain the crude product and then recrystallized to obtain 189.3 g of the pure product. The calculated yield of the product was 95.5%. The detection purity is 99.95%, the moisture content is 30ppm, and the acid value is 40ppm, and its 1H NMR spectrum is as image 3 As shown, the 13C NMR spectrum is as Figure 4 shown.

[0025] The synthetic route is:

[0026]

Embodiment 3

[0028] Add 1.0mol of propargyl alcohol and 500ml of dichloromethane into the reaction flask respectively, add triethylamine under stirring, then lower the temperature to below 15°C, start to add 2.1mol of benzenesulfonyl chloride dropwise, return to room temperature and continue stirring for 1h, then The temperature was raised to reflux to continue the reaction for 2 hours. After the reaction was completed by gas phase detection, it was ice-thawed, separated, dried and concentrated to obtain the crude product and then recrystallized to obtain 187.77 g of the pure product. The calculated yield was 95.8%. The detection purity is 99.93%, the moisture content is 28ppm, the acid value is 36ppm, and the density is 1.244g / mL.

[0029] The synthetic route is:

[0030]

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Abstract

The invention relates to a synthetic method of a benzenesulfonate derivative and belongs to the technical field of synthesis of compounds. A compound (described in the specification) is taken as raw materials, and reaction is carried out with ethylene glycol or R2-OH to generate a compound (described in the specification), wherein R1 is selected from alkyl, H or F, and R2 is selected from allyl, propargyl or benzene. The synthetic method provided by the invention comprises the following concrete operations: adding ethylene glycol or R2-OH and dichloromethane into a reactor, adding organic alkali while stirring, then cooling to the temperature below 15 DEG C, starting to dropwise add a substance (described in the specification), after the substance is dropwise added, returning to room temperature and further stirring for 0.5-1 hour, then heating and carrying out reflux reaction for 1-2 hours, after the reflux reaction is complete, carrying out ice thawing treatment, layering, drying, and concentrating, so that the benzenesulfonate derivative product is obtained. The synthetic method provided by the invention is simple, reaction process is mild and stable, yield is high, and the obtained product is high in purity.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and specifically relates to a synthesis method of benzenesulfonate derivatives. The synthesis method of the invention is simple, the reaction process is mild and stable, the yield is high, and the obtained product has high purity. Background technique [0002] With the development of my country's electronic information industry, the demand for chemical power is increasing, and its performance requirements are getting higher and higher. Lithium-ion batteries have the advantages of small size, good safety performance, light weight, high specific energy, high voltage, long life, no pollution, etc., which are incomparable to other chemical power sources. The main power supply for portable electronic devices such as camcorders and digital cameras. In recent years, the basic research and application development of lithium-ion batteries have become one of the hot spots. A lithium battery in...

Claims

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Application Information

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IPC IPC(8): C07C303/28C07C309/73H01M10/0567H01M10/42
CPCC07C303/28H01M10/0567H01M10/4235C07C309/73Y02E60/10C07C303/44
Inventor 闫彩桥刘鹏侯荣雪
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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