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A kind of preparation method of 1-propene-1,3-sultone

A technology of sultone and propylene, applied in the field of preparation of organic materials, can solve the problems of slow reaction speed and low yield of addition products, and achieve the effects of reducing waste water discharge, high product yield and fast speed

Active Publication Date: 2017-02-15
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a preparation method of 1-propene-1,3-sultone, which is used to solve the problems of slow reaction speed in the addition reaction step and low yield of addition products in the existing preparation method

Method used

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  • A kind of preparation method of 1-propene-1,3-sultone
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  • A kind of preparation method of 1-propene-1,3-sultone

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preparation example Construction

[0026] Such as figure 1 Shown: a kind of preparation method of 1-propene-1,3-sultone, comprising the following steps:

[0027] The first step, add:

[0028] Addition reaction of propargyl alcohol and alkali metal sulfite or bisulfite under the action of catalyst, propargyl alcohol and alkali metal sulfite or bisulfite are the reaction raw materials, in which: propargyl alcohol and alkali The molar ratio of metal sulfite or bisulfite is (1-10):1, the catalyst is a mixture of 2,2'-azobisisobutylamidine hydrochloride and crown ether compound, and the reaction temperature is 30-120 ℃;

[0029] The second step, acidification:

[0030] After the addition reaction is over, add inorganic acid or organic acid to stop the reaction, and the amount of acid added makes the pH value of the reaction solution reach below 4;

[0031] The third step, ring synthesis:

[0032] The acidified product is isolated, and then the 1-propene-1,3-sultone product is isolated after cyclosynthesis.

[...

Embodiment 1

[0053] Example 1, the air in the comparative example is replaced by the catalyst proposed by the present invention, wherein the molar ratio of the total amount of catalyst to the total reaction raw material is 0.0001, and 15-crown (ether)-5 and 2,2'-azo in the catalyst The molar ratio of diisobutylamidine hydrochloride is 50:1. After the addition reaction, the follow-up treatment is the same as that of the comparative example. The test results show that the reaction time is 50min, and the product 1-sulfonic acid-1-propenol is 29g. The yield is 95%.

Embodiment 2

[0054] Example 2, on the basis of Example 1, UV lamp irradiation was added, and after the addition reaction was completed, the same follow-up treatment as the comparative example was taken. The test results showed that the reaction time was 40min, and the product 1-sulfonic acid-1-propenol was 29g. The yield is 95%.

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Abstract

The invention provides a preparation method of prop-1-ene-1, 3-sultone in order to solve the problems of low reaction speed in an addition reaction step and low product yield in the existing preparation method. The preparation method comprises the following operation steps of firstly, carrying out addition reaction, namely carrying out addition reaction on reaction raw materials, namely propynol and alkali metal sulfite or bisulfite, under the action of a catalyst, wherein the molar ratio of propynol to alkali metal sulfite or bisulfite is (1-10):1, the catalyst is a mixture of 2,2'-azobis(isobutyramidine)hydrochloride and a crown ether compound, and the reaction temperature ranges from 30 DEG C to 120 DEG C; secondly, acidifying, namely adding inorganic acid or organic acid to stop the reaction after the addition reaction is ended, wherein the addition quantity of the acid is controlled according to the requirement that the pH value of a reaction solution is less than 4; and thirdly, carrying out cyclo-synthesis. The preparation method has the advantages of simplicity in operation, high reaction speed, high product yield as well as low wastewater, water gas and waste residue yield, so that the preparation method can be used for industrial application and popularization.

Description

technical field [0001] The invention relates to the technical field of preparation of organic materials, in particular to a preparation method of 1-propene-1,3-sultone. 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 200910073620.7 (publication number 101456856, publication date June 17, 2009) proposes a method for the preparation of 1-propene-1,3-sultone, using addition, acidification, and cyclosynthesis processes to prepare PST products. Wherein the specific technical scheme of the addition reaction is: the addition reaction of propargyl alcohol and alkali metal sulfite or bisulfite is carried out in aqueous solution, the addition reaction of propargyl alcohol and alkali metal sulfite o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 刘鹏梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD