Preparation method of beta-propiolactone

A technology of propiolactone and halopropionic acid, which is applied in the field of preparation of β-propiolactone, can solve the problems of complex process, high cost and unavailable raw materials of β-propiolactone, and achieve good product stability and low cost. The effect of low and simple preparation process

Pending Publication Date: 2021-09-07
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the existing technical problems of complex preparation process of β-propiolact

Method used

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  • Preparation method of beta-propiolactone

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The preparation method of β-propiolactone, comprises the steps:

[0024] (1) Dissolve 0.1mol 3-bromopropionic acid in 100mL dichloromethane at room temperature, stir and cool down to -5°C, add 0.005mol triethylamine to obtain solution A; dissolve 0.1mol potassium bicarbonate in 50mL process water, stirring and cooling down to 0°C, to obtain solution B;

[0025] (2) Mix the solution A with the solution B at 0°C under stirring, then raise the temperature to 4°C and keep it warm for 2 hours, stop stirring after the reaction is completed, cool down to 0°C and stand for 30 minutes to produce phase separation ;

[0026] (3) The organic phase obtained by phase separation is washed to neutrality with 5% mass fraction of sodium chloride aqueous solution, then cooled to -5°C, washed 2 times with process water (each 10mL process water wash), and then the washed The organic phase is dried with anhydrous magnesium sulfate, and then desolventized (removal of low-boiling dichloromet...

Embodiment 2

[0031] The preparation method of β-propiolactone, comprises the steps:

[0032] (1) Dissolve 0.1mol 3-bromopropionic acid in 100mL dichloromethane at room temperature, stir and cool down to 0°C, add 0.005mol triethylamine to obtain solution A; dissolve 0.1mol sodium bicarbonate in 50mL at room temperature In process water, stir and cool down to 0°C to obtain solution B;

[0033] (2) Mix the solution A with the solution B at 2°C under stirring, then raise the temperature to 6°C and keep it warm for 2 hours, stop stirring after the reaction is completed, cool down to 0°C and stand for 30 minutes to generate phase separation ;

[0034] (3) The organic phase obtained by phase separation is washed to neutrality with 5% mass fraction of sodium chloride aqueous solution, then cooled to -5°C, washed 2 times with process water (each 10mL process water wash), and then the washed Dry the organic matter with anhydrous magnesium sulfate, and then carry out precipitation (remove low-boili...

Embodiment 3

[0037] The preparation process of the present embodiment β-propiolactone is the same as that of Example 1, the difference is that the organic amine adopts triisopropylamine, the heat preservation reaction time of step 2 is 3h, and the yield of the present embodiment β-propiolactone product It is 80.25wt%, and the purity is 96.2wt%.

[0038] The hydrogen spectrum of the product of this embodiment is identical to that of Example 1.

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Abstract

The invention relates to a preparation method of beta-propiolactone, the preparation method comprises the following steps: (1) dissolving 3-halogenated propionic acid in an organic solvent at a room temperature, stirring, cooling to a temperature of 0 DEG C or less, and adding organic amine to obtain a solution A; preparing alkali liquor below 0 DEG C as a solution B; (2) mixing the solution A and the solution B under stirring at 0-2 DEG C, then heating to 4-6 DEG C, carrying out a heat preservation reaction, stopping stirring after the reaction is completed, cooling to 0 DEG C, and standing to generate split phases; and (3) washing the organic phase obtained by phase splitting with salt water, cooling to 0 DEG C or below, washing with water, drying, desolventizing to obtain a crude product beta-propiolactone, and distilling to obtain the product beta-propiolactone. According to the method, the reaction technology combining extraction and phase transfer is adopted, the reaction is carried out at low temperature, beta-propiolactone can be prepared at high yield, the used raw materials are easy to obtain, the cost is low, the preparation process is simple, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a preparation method of β-propiolactone. Background technique [0002] β-propiolactone, also known as beta-propiolactone, is a heterocyclic compound with a molecular number of C 3 h 4 o 2 , with a molecular weight of 72.06. It is a colorless viscous liquid at normal temperature, with a faint sweet taste and a boiling point of 162.3°C, soluble in water. Has a strong inactivation effect on viruses. It has been widely used in the inactivation of various vaccines abroad, acting on the DNA or RNA of pathogens, changing the structure of viral nucleic acid to achieve the purpose of inactivation. β-propiolactone directly interacts with viral nucleic acid instead of capsid protein, and does not destroy the immunogenicity of pathogens. Although a large dose of β-propiolactone (BPL) is a carcinogen, it is easily hydrolyzed and disappears after being hydrolyzed in a water bat...

Claims

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Application Information

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IPC IPC(8): C07D305/12
CPCC07D305/12
Inventor 吴孝兰牟新东贾自自顾小焱王聪
Owner SINOPHARM CHEM REAGENT
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