A kind of synthetic method of α-acetyl-γ-butyrolactone

A synthesis method and technology of butyrolactone, applied in the direction of organic chemistry, etc., can solve problems such as hidden dangers, difficult to implement, easy to agglomerate, etc.

Active Publication Date: 2021-09-14
LINHAI LIANSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 reaction of ethyl acetate and γ-butyrolactone through the gas phase catalysis of fluorine alkali solid-phase catalyst, although It solves the safety hazard, but due to the large energy consumption, the cost is too high, and the use of solid alkali fluoride as a catalyst has certain hidden dangers to products and environmental pollution, and has not been put into actual production and life at present.

Method used

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  • A kind of synthetic method of α-acetyl-γ-butyrolactone
  • A kind of synthetic method of α-acetyl-γ-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 method for synthesizing α-acetyl-γ-butyrolactone, comprising the following steps: after the first reaction kettle is replaced by an inert gas, metal sodium is added in an inert gas atmosphere, Warming up to the melting of sodium metal to obtain liquid sodium metal in a molten state; adding gamma-butyrolactone and acetate in the second reactor, heating up to the reflux of the system, adding dropwise liquid sodium metal in a molten state in the system, Carry out the condensation reaction, after the liquid metal sodium is added dropwise, keep the system refluxed for 1-16h; after the condensation reaction, neutralize with an acid solution, separate the phases, and obtain the α-acetyl-γ after the organic phase is distilled and rectified under reduced pressure ‑Butyrolactone. The invention adopts a solvent-free method, controls the reaction process by controlling the liquid metal sodium drop rate, has the characteristics of stable and safe reaction, and simultaneously avoids the problems of environmental pollution and difficult separation caused by using benzene substances as solvents and extractants in traditional techniques.

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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Patent Type & Authority Patents(China)
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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