Synthesis method of alpha-acetyl-gamma-butyrolactone

A synthetic method, the technology of butyrolactone, applied in the direction of organic chemistry, can solve the problems of large environmental pollution, no investment, difficult implementation, etc., and achieve the effects of eliminating pollution sources, preventing instability, and reducing production costs

Active Publication Date: 2020-02-18
LINHAI LIANSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, rapid cooling of the molten sodium metal to 50-60°C is easy to agglomerate, which is difficult to implement in industrial production, and also uses a chlorinated solvent, which causes great environmental pollution.
[0008] In addition, the Chinese patent application document (publication number: CN 101092407 A) discloses the synthesis of α-acetyl-γ-butyrolactone through the acylation re...

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The first reaction kettle is a storage tank, and the storage tank is replaced with nitrogen. In a fully dry storage tank (20L) with a thermometer and a heat-conducting oil jacket, put 3.4kg of sodium metal into it under a nitrogen atmosphere, turn on the heat-conducting oil for heating, and when the temperature reaches 130°C, keep it warm for 2 hours to make the metal All the sodium is melted to obtain liquid metallic sodium in a molten state.

[0034] The second reactor is a condensation reactor. Add 16kg of γ-butyrolactone and 49.5kg of ethyl acetate into a fully dried condensation reaction kettle (100L) equipped with an electric stirrer, a condenser, and a thermometer, stir, and then slowly heat up to raise the temperature. When the system is refluxed, open the The dripping valve of the storage tank, according to the dropping rate of 2.5kg / h, drips the liquid metal sodium in the molten state into the condensation reactor. As the dripping proceeds, the temperature in...

Embodiment 2-32

[0037] Examples 2-32: α-acetyl-γ-butyrolactone was synthesized according to the method in Example 1 using the raw materials and parameters of each example in Table 1.

[0038] Raw material parameter and result in the embodiment 1-32 of table 1

[0039]

[0040]

[0041] In summary, the synthesis method of α-acetyl-γ-butyrolactone of the present invention does not need to add benzene as a reaction solvent or extractant, and is not only safe but also has high purity and high yield, with a purity greater than 99.0% and a yield greater than 87.0%.

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Abstract

The invention relates to the technical field of chemical synthesis, and discloses a synthesis method of alpha-acetyl-gamma-butyrolactone. The method comprises: carrying out inert gas replacement on afirst reaction kettle, adding metal sodium in the inert gas atmosphere, and raising the temperature until the metal sodium is molten in order to obtain molten metal sodium; adding gamma-butyrolactoneand acetate into a second reaction kettle, raising the temperature until the system is refluxed, dropwise adding molten liquid metal sodium into the system, carrying out a condensation reaction, and keeping the system refluxed for 1-16 h after the drop-by-drop addition of the liquid metal sodium is finished; and neutralizing the system with an acid solution after the condensation reaction is finished, carrying out phase splitting, and carrying out distillation and reduced pressure rectification on the obtained organic phase to obtain the alpha-acetyl-gamma-butyrolactone. A solvent-free technology is adopted, and the reaction process is controlled by controlling the dropping speed of the liquid metal sodium, so the method has the characteristics of stable and safe reaction, and avoiding ofthe problems of environmental pollution and difficult separation caused by using benzene substances as a solvent and an extractant in the traditional process.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis method of α-acetyl-γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone is an important pharmaceutical intermediate and organic chemical raw material. It is an important intermediate for the preparation of vitamins and chlorophyll. Pharmaceutical intermediates of drugs such as thiazole, Yanxintong and chloroquine. At present, there are mainly two routes for the preparation of α-acetyl-γ-butyrolactone. One is a process based on ethylene oxide and ethyl acetoacetate as starting materials, and the other is based on γ-butyrolactone. and acetate as the starting material. [0003] Wherein, Chinese patent application documents (publication number: CN 1357545 A), U.S. Patent US 2443827, British Patent GB 740993 and Japanese Patent JP 4212662 etc. all disclose similar synthesis of starting materials with ethylene oxide and ethyl acetoacetate Pr...

Claims

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Application Information

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IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 强永康黄卫国崔峰巍李生黄斌姚素
Owner LINHAI LIANSHENG CHEM
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