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Preparation method of 1-propene-1,3-sultone

A technology of sultone and propylene, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve problems such as restricting development, and achieve faster reaction speed and improved product purity. Effect

Pending Publication Date: 2022-01-14
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the eyes of those skilled in the art, the change of the catalyst can only change the rate of the reaction, and due to the many reaction links, the change of the catalyst is likely to produce unnecessary impurities in the later reaction, so those skilled in the art generally will not Making a fuss about catalysts also restricts the development of this product

Method used

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  • Preparation method of 1-propene-1,3-sultone
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  • Preparation method of 1-propene-1,3-sultone

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preparation example Construction

[0011] A preparation method of 1-propene-1,3-sultone, comprising carrying out addition reaction with propargyl alcohol and alkali metal sulfite or bisulfite under the action of a catalyst, adding Inorganic acid or organic acid is acidified, and the acidified product is separated, and then the cyclosynthesis reaction is carried out, and the 1-propene-1,3-sultone product is separated again. The key is: the catalyst in the addition reaction The components are composed by mass percentage: 60-80% of onium salt and 20-40% of crown ether.

[0012] The onium salt is trimethylbenzyl ammonium chloride, or tetrabutylammonium bisulfate, or a mixture of the above two substances.

[0013] The crown ether is 18-crown ether-6 with a solubility of 5-10%.

[0014] After the acidification process is finished, the pH value of the reaction solution is controlled to reach 3.5-3.8.

[0015] The molar ratio of propargyl alcohol to alkali metal sulfite or bisulfite is (1-10):1.

[0016] The reactio...

Embodiment 1

[0025] The catalyst air in the comparative example was replaced with 80ml of trimethylbenzyl ammonium chloride and 20ml of 18-crown-6. The test results showed that the reaction time was 35min, the yield was 98%, and the purity could reach chemical purity.

Embodiment 2

[0027] The catalyst air in the comparative example was replaced with 60ml of trimethylbenzyl ammonium chloride and 40ml of 18-crown-6. The test results showed that the reaction time was 36min, the yield was 97%, and the purity could reach chemical purity.

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Abstract

The invention discloses a preparation method of 1-propene-1,3-sultone. The preparation method comprises the following steps: carrying out an addition reaction on propargyl alcohol and alkali metal sulfite or hydrosulfite under the action of a catalyst, adding inorganic acid or organic acid for acidification after the addition reaction is finished, separating out an acidified product, then carrying out cyclization reaction and carrying out separation to obtain a 1-propene-1,3-sultone product. The method is characterized in that the catalyst in the addition reaction comprises the following components in percentage by mass: 60 to 80 percent of onium salt and 20 to 40 percent of crown ether. The method has the beneficial effects that by changing the type of the catalyst, the reaction speed of the 1-propene-1,3-sultone product is greatly increased, yield reaches 98%, and meanwhile, product purity is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic materials, and relates to a preparation method of 1-propene-1,3-sultone, in particular to a preparation method which can greatly improve product quality. Background technique [0002] 1-propene-1,3-sultone (referred to as PST) is an important pharmaceutical intermediate. Its unique structure makes it irreplaceable in the synthesis of heterocyclic drugs. It can also be used as lithium Additives for battery electrolyte, used to prolong the service life of lithium batteries. [0003] Patent ZL201310511144.9 is an invention patent applied by our company in the early years, and the product quality has been relatively stable all the time. However, with the continuous update of downstream customer needs and increasingly fierce market competition, the original product yield and quality can no longer be satisfied. Our technicians found that the selection and use of catalysts may play a dec...

Claims

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Application Information

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IPC IPC(8): C07D327/04B01J31/02
CPCC07D327/04B01J31/0239B01J31/0204
Inventor 田丽霞张茜葛建民郝俊赵光华刘鹏
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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