Synthetic method for ethylene sulfite derivative

A vinyl sulfite and synthesis method technology, applied in the direction of organic chemistry, can solve the problems of many by-products, low yield, poor safety, etc., achieve high conversion rate of raw materials, high product yield, and increase reaction conversion rate and the effect of the yield

Inactive Publication Date: 2018-05-04
LIAONING KELONG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And at present, the problem that is used to prepare the method for vinyl sulfite derivative to exist is: 1, prepare by reaction of thionyl chloride and corresponding diol
However, the operating conditions of this method require high temperature and high pressure, poor safety, many by-products and low yield.

Method used

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  • Synthetic method for ethylene sulfite derivative
  • Synthetic method for ethylene sulfite derivative
  • Synthetic method for ethylene sulfite derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The synthesis of embodiment 1 vinyl sulfite

[0024] In a three-neck flask equipped with a condenser, a stirrer and a thermometer, add 1000 g of ethylene glycol and 10 g of calcium oxide, and react at 110° C. for 2 hours. In order to prevent water vapor in the air from entering, a drying tube is added to the top of the condensation tube, and anhydrous magnesium sulfate is added into the drying tube. Then vacuum rapid filtration, the water content is 100ppm with trace moisture analyzer.

[0025] In a three-necked flask equipped with a stirrer, a thermometer, and a fractionating tower, add 620 g of dried ethylene glycol, add 8.6 g of tetraisopropyl titanate, react at 120 ° C for 1 hour, and then add 1100 g of dimethyl sulfite , start the reaction when the oil bath is 120°C, and keep the fractionation tower top temperature at 64-67°C by controlling the oil bath temperature not to exceed 150°C. When the temperature of the oil bath was at 150° C. and methanol was no longer...

Embodiment 2

[0028] Example 2 Synthesis of 4,5-dimethyl vinyl sulfite

[0029] Add 900g of 2,3-butanediol and 13g of anhydrous magnesium sulfate into a three-neck flask equipped with a condenser, a stirrer and a thermometer, and react at 120°C for 2 hours. In order to prevent water vapor in the air from entering, a drying tube is added to the top of the condensation tube, and anhydrous magnesium sulfate is added into the drying tube. Vacuum fast filtration then, measure water content with trace moisture meter and be 150ppm.

[0030] In a three-neck flask equipped with a stirrer, a thermometer, and a fractionating tower, add 472 g of dried 2,3-butanediol, add 10 g of n-propyl titanate, react at 120 ° C for 1.5 hours, and then add 550 g of disulfite Methyl esters start to react when the oil bath is 120°C, and by controlling the temperature of the oil bath not to exceed 150°C, the temperature at the top of the fractionation column is kept at 64-67°C. When the temperature of the oil bath was...

Embodiment 3

[0033] Example 3 4-butyl vinyl sulfite

[0034] Add 1000g of 1,2-hexanediol and 15g of anhydrous sodium sulfate into a three-necked flask equipped with a condenser, stirring and thermometer, and react at 130°C for 2 hours. In order to prevent water vapor in the air from entering, a drying tube is added to the top of the condensation tube, and anhydrous magnesium sulfate is added into the drying tube. Vacuum fast filtration then, measure water content with trace moisture meter and be 180ppm.

[0035] In a three-necked flask equipped with a stirrer, a thermometer, and a fractionating tower, add 594 g of dried 1,2-hexanediol, add 11 g of tetrabutyl titanate, react at 120 ° C for 2 hours, and then add 550 g of disulfite Methyl esters start to react when the oil bath is 120°C, and by controlling the temperature of the oil bath not to exceed 150°C, the temperature at the top of the fractionation column is kept at 64-67°C. When the temperature of the oil bath was at 150° C. and met...

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Abstract

The invention relates to a synthetic method for an ethylene sulfite derivative, and belongs to the field of fine chemical synthesis. The synthetic method comprises the following steps: with titanate as a catalyst, carrying out ester exchange on dimethyl sulfite and corresponding glycol to synthesize the target compound, wherein the using amount of the catalyst is 0.01% to 2% of total weight of reactants, and the mole ratio of the used glycol to the used dimethyl sulfite is 1 to 1.2; reacting at the temperature of 80 to 150 DEG C, gradually carrying out fractionation to remove generated methylalcohol, and stopping the reaction when the methyl alcohol is not fractionated any longer; and carrying out vacuum distillation on the reaction product, and collecting the target substance. The methodhas the advantages of no corrosion, high raw material conversion rate, high yield and the like.

Description

technical field [0001] The invention relates to the field of fine chemical synthesis, in particular to a synthesis method of vinyl sulfite derivatives. Background technique [0002] Vinyl sulfite derivatives are an important organic chemical product, which can be used as an organic solvent for the electrolyte of lithium-ion batteries, and can also be used as an additive for the electrolyte of lithium-ion batteries. After adding vinyl sulfite to the electrolyte of lithium-ion batteries, it will appear Excellent storage stability can improve the low-temperature performance of the electrolyte. With the vigorous development of the lithium-ion battery industry, the requirements for battery performance are getting higher and higher, and the demand for vinyl sulfite derivatives as an excellent solvent or additive also increases accordingly. Vinyl sulfite derivatives can also be used in organic synthesis and pharmaceutical intermediates. At present, the problems existing in the me...

Claims

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Application Information

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IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 王炳帅姜艳
Owner LIAONING KELONG FINE CHEM
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