Preparation method of α-acetyl-γ-butyrolactone

A technology of butyrolactone and acetyl group, applied in the field of preparation of α-acetyl-γ-butyrolactone, can solve the problems of less than 85%, low yield and the like, and achieves reduction of hydrolysis, simple separation system, and elimination of containing Effect of Phosphorus Wastewater and Waste Salt

Active Publication Date: 2022-08-05
江西天新药业股份有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 α-acetyl-γ-butyrolactone
  • Preparation method of α-acetyl-γ-butyrolactone
  • Preparation method of α-acetyl-γ-butyrolactone

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preparation example Construction

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

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

[0024] (2) in the presence of water, make the material containing α-acetyl-γ-butyrolactone sodium salt and CO 2 The neutralization reaction occurs when the gas contacts.

[0025] According to the method of the present invention, preferably, in step (1), R 1 and R 2 Each independently is preferably 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 reflux and distillation device, and the re...

Embodiment 1

[0054] (1) Acylation reaction: The reaction was carried out in a dry 50L stainless steel reaction tank equipped with stirring, refluxing and distillation devices. Turn on 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 methoxide in batches, keep the system temperature at 43°C to between 48°C. The reaction system was gradually heated to 55°C, slowly opened the valve of the distillation unit, controlled the reflux ratio to be 4:1, and collected about 20 kg of the mixture of methanol and methyl acetate generated by the reaction, which was used for rectification, separation and recovery. At the same time, 10.3 kg of methyl acetate was slowly added, the temperature was slowly increased, the pressure in the tank was 0.15 MPa, and the reaction was maintained at 85 ° C for 5 h. About 1% of γ-butyrolactone remained in the reaction system by gas chromatogr...

Embodiment 2

[0059] (1) Acylation reaction: The reaction was carried out in a dry 50L stainless steel reaction tank equipped with stirring, refluxing and distillation devices. Turn on 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 methoxide in batches, keep the system temperature at 43°C to between 48°C. The reaction system was gradually heated to 55°C, slowly opened the valve of the distillation unit, controlled the reflux ratio to be 4:1, and collected about 20 kg of the mixture of methanol and methyl acetate generated by the reaction, which was used for rectification, separation and recovery. At the same time, 7.5 kg of methyl acetate was slowly added, the temperature was slowly increased, the pressure in the tank was 0.15 MPa, and the reaction was maintained at 88 °C for 3 hours. The reaction system was monitored by gas chromatography about 3% of γ-butyr...

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Abstract

The invention relates to the field of organic synthesis, and discloses a preparation method of α-acetyl-γ-butyrolactone, which comprises the following steps: (1) making γ-butyrolactone, CH 3 COOR 1 and R 2 ONa undergoes acylation reaction to obtain the material containing α-acetyl-γ-butyrolactone sodium salt, wherein R 1 and R 2 Each independently is an alkyl group of C1-C4; (2) in the presence of water, make the material containing α-acetyl-γ-butyrolactone sodium salt and CO 2 The neutralization reaction occurs when the gas contacts. The method provided by the invention also has the advantage of higher yield under the condition of ensuring safety, which provides convenience for the large-scale production of α-acetyl-γ-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 in the production and preparation of various drugs. There are two main process routes at present: one is the process route of ring-opening and re-esterification of ethylene oxide with methyl acetoacetate (or ethyl) ester; the other is the use of γ-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 acetoacetate (or ethyl) ester route is 10.8°C, which is a first-class flammable and explosive chemical, which will cause serious safety hazards for storage, transportation and production. This process route is gradually eliminated, and the mainstream production of domestic enterpr...

Claims

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Application Information

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Patent Type & Authority Patents(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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