Method for preparing alpha-acetyl-gamma-butyrolactone

A technology of butyrolactone and acetyl, which is applied in the field of preparing α-acetyl-γ-butyrolactone, can solve the problems of cumbersome operation and environmental pollution, and achieve the effects of simple operation, easy-to-obtain raw materials and high yield

Inactive Publication Date: 2018-10-16
陈正新
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route has the advantages of high yield and low cost, but there are still problems of cumbersome operation and serious environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for preparing α-acetyl-γ-butyrolactone, comprising the steps of: adding 80 parts of ethyl acetate and 45 parts of sodium carbonate to a three-necked flask, adding 40 parts of γ-butyrolactone dropwise at 45°C, Stir for 45 minutes, uniformly mix 55 parts of ethyl acetate and 35 parts of liquid acetaldehyde, add the reaction solution dropwise within 2 hours, mix evenly, stir and react at 56°C for 2 hours, put the reaction solution into an autoclave at 82°C and keep it warm for 5.5 hours. After the reaction, pass water to cool down to room temperature, add the reaction solution into a four-necked bottle, wash the autoclave with 25 parts of ethyl acetate, and incorporate the washing solution into the reaction solution, and slowly add the reaction solution at 4°C with a mass fraction of 65% Sulfuric acid was used to adjust the pH to 6.5. During the dropwise addition, solids were precipitated. After the dropwise addition, stirred at 30°C for 12 hours. The pH remained u...

Embodiment 2

[0021] A method for preparing α-acetyl-γ-butyrolactone, comprising the steps of: adding 75 parts of ethyl acetate and 40 parts of sodium carbonate to a three-necked flask, adding 35 parts of γ-butyrolactone dropwise at 44°C, Stir for 40 minutes, mix 50 parts of ethyl acetate and 30 parts of liquid acetaldehyde evenly, add the reaction solution dropwise within 1.5 hours, mix well and then stir and react at 54°C for 1.5 hours, then put the reaction solution into an autoclave at 80°C and keep it warm for 5 hours After the reaction, cool down to room temperature with water, add the reaction solution into a four-necked bottle, wash the autoclave with 20 parts of ethyl acetate, and incorporate the washing solution into the reaction solution, and slowly dropwise add a mass fraction of 65 at 3°C. % sulfuric acid to adjust the pH to 6, during the dropwise addition, solids were precipitated, after the dropwise addition, stirred at 25°C for 11h, re-measured the pH unchanged, filtered to r...

Embodiment 3

[0023] A method for preparing α-acetyl-γ-butyrolactone, comprising the steps of: adding 85 parts of ethyl acetate and 50 parts of sodium carbonate to a three-necked flask, adding 45 parts of γ-butyrolactone dropwise at 46°C, Stir for 50 minutes, mix 60 parts of ethyl acetate and 40 parts of liquid acetaldehyde evenly, add the reaction solution dropwise within 2.5 hours, mix well, stir and react at 58°C for 2.5 hours, put the reaction solution into an autoclave at 85°C and keep it warm for 6 hours , after the reaction was completed, cool down to room temperature with water, add the reaction solution into a four-necked bottle, wash the autoclave with 30 parts of ethyl acetate, and incorporate the washing solution into the reaction solution, and slowly dropwise add a mass fraction of 65% at 5°C. % sulfuric acid to adjust the pH to 7, and solids were precipitated during the dropwise addition. After the dropwise addition, stirred at 35°C for 13h, and the pH remained unchanged after ...

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Abstract

The invention discloses a method for preparing alpha-acetyl-gamma-butyrolactone. The method comprises the following steps: adding ethyl acetate and sodium carbonate into a three-necked flask, dropwiseadding gamma-butyrolactone at the temperature of 44 to 46 DEG C, stirring, mixing the ethyl acetate and liquid aldehyde, dropwise adding a reaction solution, uniformly mixing, stirring and reacting for 1.5 to 2.5 hours at the temperature of 54 to 58 DEG C, adding the reaction solution into a high-pressure kettle, reacting for 5 to 6 hours at the temperature of 80 to 85 DEG C, cooling to room temperature, adding the reaction solution into a three-necked flask, dropwise adding sulfuric acid at 3 to 5 DEG C to adjust the pH to be 6 to 7, precipitating solids in the dropwise addition process, after the addition is ended, stirring for 11 to 13 hours, re-testing the pH which is unchanged, filtering to remove the solids, washing a filter cake by using ethyl acetate, performing the decompressionrotary evaporation, removing the ethyl acetate until no fraction is outputted, obtaining a crude product, and performing the direct decompression rectification for the crude product. The preparation method is easy in obtaining raw materials, cheap in raw materials, easy in operation, higher in yield, and suitable for industrialized production.

Description

technical field [0001] The present invention relates to a method for preparing α-acetyl-γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone (English name α-acetyl-γ-butyrolactone) is a colorless and transparent liquid with an ester odor, CAS No. 517-23-7. α-acetyl-γ-butyrolactone can be used in the analysis of primary amines or sulfa drugs through color reaction, and it is also a widely used chemical intermediate, often used in the synthesis of vitamin B1, antipsychotic drugs risperidone, Anticonvulsant and sedative-hypnotic drugs such as chlormethiazide hydrochloride, chlorophyll, Yanxintong, chloroquine, 3-mercapto-4-oxo-pentyl acetate, cyproamine, fungicide prothioconazole and other drugs. [0003] At present, there are two main synthetic routes for α-acetyl-γ-butyrolactone: γ-butyrolactone and ethyl acetate are used as raw materials, and a strong base is used as a condensing agent, which is prepared by Claisen condensation; the other uses alcohol as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 陈正新
Owner 陈正新
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