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Preparation method of alpha-acetyl-gamma-butyrolactone

A technology of butyrolactone and acetyl, which is applied in the field of preparation of α-acetyl-γ-butyrolactone, can solve the problems of low yield, less than 85%, achieve simple separation system, reduce hydrolysis and side reactions little effect

Active Publication Date: 2020-09-04
江西天新药业股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Said method adopts sodium methylate to replace metallic sodium, has solved the safety problem existing because of using metallic sodium, but the yield of said method is all low, all less than 85%

Method used

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

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preparation example Construction

[0022] The present invention provides a kind of preparation method of α-acetyl-γ-butyrolactone, the method comprises the following steps:

[0023] (1) Make γ-butyrolactone, CH 3 COOR 1 and R 2 ONa undergoes acylation reaction to obtain a material containing α-acetyl-γ-butyrolactone sodium salt, wherein R 1 and R 2 Each is independently a C1-C4 alkyl group;

[0024] (2) Under the condition that water exists, make the material containing α-acetyl-γ-butyrolactone sodium salt and CO 2 A neutralization reaction occurs on gas contact.

[0025] According to the method of the present invention, preferably, in step (1), R 1 and R 2 Each independently preferably is a C1-C2 alkyl group such as methyl, ethyl. R 1 and R 2 Can be the same or different.

[0026] According to the method of the present invention, in step (1), the acylation reaction is generally carried out under dry conditions, and the acylation reaction is preferably carried out in a reaction tank equipped with a r...

Embodiment 1

[0054] (1) Acylation reaction: the reaction is carried out in a dry 50L stainless steel reaction tank equipped with stirring, reflux and distillation devices. Turn on the stirring, replace the reaction tank with nitrogen, add 20.7kg of methyl acetate, raise the temperature in the reaction tank to 45°C, add 4kg of γ-butyrolactone and 2.6kg of sodium methylate in batches, and keep the system temperature at 43°C to between 48°C. Gradually raise the temperature of the reaction system to 55°C, slowly open the valve of the distillation device, control the reflux ratio to 4:1, collect about 20kg of the mixture of methanol and methyl acetate generated in the reaction, and use it for rectification, separation and recovery. At the same time, 10.3kg of methyl acetate was added slowly, the temperature was raised slowly, the pressure inside the tank was 0.15MPa, and the pressure was maintained at 85°C for 5h. About 1% of γ-butyrolactone remains in the reaction system monitored by gas chro...

Embodiment 2

[0059] (1) Acylation reaction: the reaction is carried out in a dry 50L stainless steel reaction tank equipped with stirring, reflux and distillation devices. Turn on the stirring, replace the reaction tank with nitrogen, add 20.7kg of methyl acetate, raise the temperature in the reaction tank to 45°C, add 4kg of γ-butyrolactone and 2.6kg of sodium methylate in batches, and keep the system temperature at 43°C to between 48°C. Gradually raise the temperature of the reaction system to 55°C, slowly open the valve of the distillation device, control the reflux ratio to 4:1, collect about 20kg of the mixture of methanol and methyl acetate generated in the reaction, and use it for rectification, separation and recovery. At the same time, 7.5 kg of methyl acetate was added slowly, the temperature was raised slowly, the pressure in the tank was 0.15 MPa, and the pressure was kept at 88° C. for 3 h. About 3% of γ-butyrolactone remains in the reaction system monitored by gas chromatogr...

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Abstract

The invention relates to the field of organic synthesis, and discloses a preparation method of alpha-acetyl-gamma-butyrolactone. The method comprises the following steps: (1) gamma-butyrolactone, CH3COOR1 and R2ONa are subjected to acylation reaction to obtain a material containing alpha-acetyl-gamma-butyrolactone sodium salt, and R1 and R2 are respectively independently C1-C4 alkyl; and (2) in the presence of water, the material containing the alpha-acetyl-gamma-butyrolactone sodium salt is enabled to be in contact with CO2 gas to generate neutralization reaction. The method also has the advantage of higher yield under the condition of ensuring safety, and provides convenience for large-scale production of alpha-acetyl-gamma-butyrolactone.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of α-acetyl-γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone is an important intermediate in the field of pharmaceutical and chemical production, which can be used to produce a variety of drugs. There are mainly two kinds of current process routes: one is the process route of ring-opening and re-esterifying ring-closing of ethylene oxide with methyl (or ethyl) acetoacetate; the other is to use gamma-butyrolactone and methyl acetate (or ethyl) ester is the acylation process route of raw material. The boiling point of ethylene oxide used in the methyl (or ethyl) acetoacetate route is 10.8°C, which belongs to the first-class flammable and explosive chemicals, which will cause serious safety hazards in storage, transportation, and production links. Therefore, the current This process route has been eliminated gradually, and the mainstream...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 郭官安李全国袁玉坤夏雨万挺峰司玉贵
Owner 江西天新药业股份有限公司
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