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
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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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