Synthesis method for alpha-acetyl gamma-butyrolactone

A synthetic method and technology of butyrolactone, applied in the direction of organic chemistry, can solve the problems of high production cost, low purity of α-acetyl γ-butyrolactone, etc., and achieve the effect of mild reaction conditions

Inactive Publication Date: 2018-03-30
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the synthetic method of α-acetyl γ-butyrolactone provided by the prior art also

Method used

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  • Synthesis method for alpha-acetyl gamma-butyrolactone
  • Synthesis method for alpha-acetyl gamma-butyrolactone

Examples

Experimental program
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Effect test

Embodiment 1

[0023] A kind of synthetic method of α-acetyl gamma-butyrolactone, the synthetic method of this α-acetyl gamma-butyrolactone comprises the following steps:

[0024] (1) Slowly heat up the reactor to 75°C, add γ-butyrolactone, ethyl acetate and sodium ethoxide, and reflux for 10 hours to obtain the sodium salt of α-acetyl-γ-butyrolactone and by-product ethanol, Wherein, the molar ratio of gamma-butyrolactone and ethyl acetate is 1:3, and the molar ratio of gamma-butyrolactone and sodium ethylate is 1:1.4;

[0025] (2) Distill the product obtained in step (1), remove ethanol and excess ethyl acetate, adjust the pH to 3 with dilute sulfuric acid for the residue, let stand to separate the liquid and separate the water phase, the organic phase is at a pressure of -0.1Mpa, and the temperature α-acetyl γ-butyrolactone was obtained by distillation under reduced pressure at 65°C.

Embodiment 2

[0027] A kind of synthetic method of α-acetyl gamma-butyrolactone, the synthetic method of this α-acetyl gamma-butyrolactone comprises the following steps:

[0028] (1) Slowly heat up the reactor to 75°C, add γ-butyrolactone, ethyl acetate and sodium ethoxide, and reflux for 10 hours to obtain the sodium salt of α-acetyl-γ-butyrolactone and by-product ethanol, Wherein, the molar ratio of gamma-butyrolactone and ethyl acetate is 1:5, and the molar ratio of gamma-butyrolactone and sodium ethylate is 1:1.2;

[0029] (2) The product obtained in step (1) is distilled to remove ethanol and excess ethyl acetate, and the residue is adjusted to pH 4 with dilute sulfuric acid, and left to stand for liquid separation to remove the water phase. Under the condition of 70°C, carry out vacuum distillation to obtain α-acetyl γ-butyrolactone.

Embodiment 3

[0031] A kind of synthetic method of α-acetyl gamma-butyrolactone, the synthetic method of this α-acetyl gamma-butyrolactone comprises the following steps:

[0032] (1) Slowly heat up the reactor to 75°C, add γ-butyrolactone, ethyl acetate and sodium ethoxide, and reflux for 10 hours to obtain the sodium salt of α-acetyl-γ-butyrolactone and by-product ethanol, Wherein, the molar ratio of gamma-butyrolactone and ethyl acetate is 1:3, and the molar ratio of gamma-butyrolactone and sodium ethylate is 1:1.6;

[0033] (2) Distill the product obtained in step (1), remove ethanol and excess ethyl acetate, adjust the pH to 3 with dilute sulfuric acid for the residue, let stand to separate the liquid and separate the water phase, the organic phase is at a pressure of -0.1Mpa, and the temperature α-acetyl γ-butyrolactone was obtained by distillation under reduced pressure at 66°C.

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Abstract

The invention relates to the field of synthesis of organic intermediates of prothioconazole, in particular to a synthesis method for alpha-acetyl gamma-butyrolactone. The synthesis method includes thefollowing steps of (1) slowly heating a reactor to 75 DEG C, and adding gamma-butyrolactone, ethyl acetate and sodium ethoxide for reflux reaction for 10 hours to obtain a sodium salt of alpha-acetylgamma-butyrolactone and a by-product ethanol; (2) distilling the product obtained in the step (1) to remove the ethanol and excess ethyl acetate, adjusting the pH of the residue to 3-4 with dilute sulfuric acid, standing for liquid separation, removing aqueous phase, and performing vacuum distillation in an organic phase at a pressure of 0.1 MPa and a temperature of 65-70 DEG C to obtain alpha-acetyl gamma-butyrolactone. The synthesis method uses a reaction base material ethyl acetate as a base solvent and uses sodium ethoxide as a condensing agent, has mild reaction conditions and improved safety, avoids pollution caused by adopting additional solvents such as benzene solvent and the like, and has good safety, simple post-treatment method, high yield of alpha-acetyl gamma-butyrolactone above 90%, and high purity of alpha-acetyl gamma-butyrolactone above 98%.

Description

technical field [0001] The invention relates to the field of synthesis of prothioconazole organic intermediates, in particular to a synthesis method of α-acetyl γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone is an important organic chemical raw material. It is a raw material for the preparation of vitamins (mainly used for the synthesis of vitamin B1) and an intermediate of chlorophyll. It can also be used in the pharmaceutical industry to manufacture anti-anginal drugs. Heartache and other drugs can also be synthesized with 3,4-disubstituted pyridine and 5-(β-hydroxyethyl)-4-methylthiazole. [0003] At present, there are mainly two methods for synthesizing α-acetyl-γ-butyrolactone at home and abroad. One is to use γ-butyrolactone and ethyl acetate as starting materials, and use metal sodium as a condensation agent to prepare target product. However, metal sodium is used in this synthetic route to participate in the reaction, and the reaction is to...

Claims

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Application Information

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IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 吴海峡张宇张财华张志宏周爱民
Owner ANHUI COSTAR BIOCHEM CO LTD
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