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Application of liquid sodium methoxide in synthesis of alpha-acetyl-gamma-butyrolactone and synthesis method of alpha-acetyl-gamma-butyrolactone

A synthetic method and technology of butyrolactone, applied in the direction of organic chemistry, can solve the problems of high fire risk, large body injury, easy moisture absorption and spontaneous combustion of solid sodium methoxide, etc., and achieve the effect of reducing the risk of feeding

Active Publication Date: 2021-05-07
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The raw material used in the acylation process of the existing α-acetyl-γ-butyrolactone synthesis is solid sodium methoxide, which needs to be manually fed into the reactor. Because solid sodium methoxide is easy to absorb moisture and spontaneously ignite, the risk of fire is relatively high
Solid sodium methoxide is easy to raise dust, and the dust is relatively large during the feeding process, which will cause great harm to employees if inhaled

Method used

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  • Application of liquid sodium methoxide in synthesis of alpha-acetyl-gamma-butyrolactone and synthesis method of alpha-acetyl-gamma-butyrolactone

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[0055] According to the second aspect of the present invention, a kind of synthetic method of α-acetyl-γ-butyrolactone is provided, comprising the following steps:

[0056] In the presence of liquid sodium methoxide, catalyzing the acylation reaction of acetate compounds and γ-butyrolactone to synthesize α-acetyl-γ-butyrolactone.

[0057] The present invention uses liquid sodium methoxide instead of solid sodium methoxide for acylation synthesis, realizes liquefaction and sealing of feeding, and reduces the risk of on-site feeding. Moreover, the synthetic yield of α-acetyl-γ-butyrolactone can be increased from 89% to over 96%.

[0058] Acetate compounds include, but are not limited to, methyl acetate (methyl acetate), ethyl acetate, and the like.

[0059] Specifically, the synthetic method of α-acetyl-γ-butyrolactone comprises the following steps:

[0060] (a) Acetate compound and gamma-butyrolactone carry out pre-acylation reaction;

[0061] Preferably, the mass ratio of a...

Embodiment 1

[0086] A preparation method of α-acetyl-γ-butyrolactone, comprising the following steps:

[0087] Mix 100g of methyl acetate and 100g of γ-butyrolactone in a flask, and react for 4 hours at room temperature at about 25°C. After the reaction is completed, continue to add 235g of liquid sodium methoxide into the flask, and continue to stir and react for 1 hour. Quantitatively concentrate 160g of methanol, transfer the material into the acylation kettle, and continue to add 150g of methyl acetate into the acylation kettle, and keep the temperature at about 85°C for 3 hours to carry out the acylation reaction. After the reaction was finished, the temperature was lowered out of the still, neutralized with 85g of acetic acid, and the crude product of sodium acetate and butyrolactone was obtained after filtration. The lactone content is 72% (detected by gas phase GC), and the reaction yield is 92.6%.

Embodiment 2

[0089] A preparation method of α-acetyl-γ-butyrolactone, comprising the following steps:

[0090] Mix 100g of methyl acetate and 100g of γ-butyrolactone in a flask, and react for 4 hours at room temperature at about 25°C. After the reaction, continue to add 250g of liquid sodium methoxide into the flask, and continue to stir and react for 1 hour. Quantitatively concentrate 170g of methanol, transfer the material into the acylation kettle, and continue to add 150g of methyl acetate into the acylation kettle, and keep the temperature at about 85°C for 3 hours to carry out the acylation reaction. After the reaction was completed, the temperature was lowered out of the kettle, neutralized with 88.9g of acetic acid, and the crude product of sodium acetate and butyrolactone was obtained after filtration. The lactone content is 73.6%, and the reaction yield is 94.1%.

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Abstract

The invention provides application of liquid sodium methoxide in synthesis of alpha-acetyl-gamma-butyrolactone and a synthesis method of the alpha-acetyl-gamma-butyrolactone, and relates to the technical field of organic synthesis. The synthesis method of the alpha-acetyl-gamma-butyrolactone comprises the following steps: (a) performing pre-acylation reaction on an acetate compound and gamma-butyrolactone; (b) adding liquid sodium methoxide into the reaction liquid in the step (a) to carry out mixed reaction; (c) after the reaction in the step (b) is finished, concentrating and collecting methanol, and transferring the concentrated reaction liquid into an acylation kettle; (d) supplementing the acetate compound into the acylation kettle for acylation reaction; (e) performing neutralizing, filtering and concentrating to obtain an alpha-acetyl-gamma-butyrolactone crude product. According to the method, liquid sodium methoxide is used for replacing solid sodium methoxide for acylation synthesis, so that liquification and sealing of feeding are realized, the on-site feeding risk is reduced, and the synthesis yield is increased to 96% or above.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to the application of liquid sodium methoxide in the synthesis of α-acetyl-γ-butyrolactone and the synthesis method of α-acetyl-γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone (ABL) is an important pharmaceutical intermediate and organic chemical raw material. The commonly used reaction route is: in the presence of a strong base (metal sodium, metal potassium, sodium alkoxide, sodium amide, etc.), catalyze the acylation reaction of ethyl acetate and γ-butyrolactone to synthesize α-acetyl-γ-butyrolactone ester. [0003] The raw material used in the existing α-acetyl-γ-butyrolactone synthesis and acylation process is solid sodium methoxide, which needs to be manually fed into the reactor. Because solid sodium methoxide is easy to absorb moisture and spontaneously ignite, the risk of fire is relatively high. Solid sodium methoxide is easy to raise du...

Claims

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Application Information

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IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 徐晓海李褦成陈英明严建斌
Owner 江苏兄弟维生素有限公司
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