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Method for preparing alpha-acetyl-gamma-butyrolactone

A technology of butyrolactone and butyrolactone sodium salt, applied in the direction of organic chemistry and the like, can solve the problems of high energy consumption, long purification cycle and high equipment requirements, and achieve the effects of low energy consumption, short purification time and high product purity

Inactive Publication Date: 2018-06-08
NORTHEAST PHARMA GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of α-acetyl-γ-butyrolactone by the above method has many disadvantages such as long purification cycle, high energy consumption, and high requirements for equipment.

Method used

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  • Method for preparing alpha-acetyl-gamma-butyrolactone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 100g of ethyl acetate into a 500ml reaction flask, heat up to 50°C, and simultaneously add 80g of solid sodium methoxide and the mixture, which is formed by mixing 86g of ethyl acetate and 100g of γ-butyrolactone. Keep the system temperature at 50°C and complete the addition within 2 hours. After the material was added, stirring was continued rapidly at 60° C. for 1 h. For discharging, add the above reaction solution into a 500ml autoclave, and conduct a high-pressure reaction at 100°C for 2 hours. The pressure gauge shows that the pressure is small, and the pressure range is 0.1-1MPa. After the reaction is completed, cool down, discharge, and use 20g of ethyl acetate to wash the reaction Kettle, the washing solution was combined into the reaction solution for use. Transfer the above materials to a 500ml reaction flask, distill under reduced pressure at 50°C (vacuum degree 0.09MPa—0.1MPa), concentrate to near dryness, and the precipitated solid is α-acetyl-γ-butyro...

Embodiment 2

[0020] Add 100g of ethyl acetate into a 500ml reaction flask, heat up to 50°C, add 80g of solid sodium methoxide and the mixed solution at the same time, the mixed solution is formed by mixing 86g of ethyl acetate and 100g of γ-butyrolactone, keep the system temperature at 50°C, Added within 2h. After the material was added, stirring was continued rapidly at 60° C. for 1 h. For discharging, add the above-mentioned liquid materials into a 500ml autoclave, and conduct a high-pressure reaction at 100°C for 2 hours. The pressure gauge shows that the pressure is small, and the pressure range is 0.1-1MPa. After the reaction is completed, cool down, discharge, and use 20g of ethyl acetate to wash the reaction Kettle, the washing solution was combined into the reaction solution for use. The above material was transferred to a 500ml reaction flask, distilled under reduced pressure at 60°C (vacuum degree 0.09MPa—0.1MPa), concentrated to near dryness, and the precipitated solid was α-ac...

Embodiment 3

[0023] Add 100g of ethyl acetate into a 500ml reaction flask, heat up to 50°C, add 80g of solid sodium methoxide and the mixed solution at the same time, the mixed solution is formed by mixing 86g of ethyl acetate and 100g of γ-butyrolactone, keep the system temperature at 50°C, Added within 2h. After the material was added, stirring was continued rapidly at 60° C. for 1 h. For discharging, add the above-mentioned liquid materials into a 500ml autoclave, and conduct a high-pressure reaction at 100°C for 2 hours. The pressure gauge shows that the pressure is small, and the pressure range is 0.1-1MPa. After the reaction is completed, cool down, discharge, and use 20g of ethyl acetate to wash the reaction Kettle, the washing solution was combined into the reaction solution for use. The above materials were transferred to a 500ml reaction flask, distilled under reduced pressure at 60°C (vacuum degree 0.09MPa—0.1MPa), concentrated to near dryness, and α-acetyl-γ-butyrolactone sodi...

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Abstract

The invention discloses a method for preparing alpha-acetyl-gamma-butyrolactone and relates to the technical field of chemical product preparation. The method comprises the following steps: by takingsolid sodium methoxide as a catalyst and gamma-butyrolactone and ethyl acetate as initial raw materials, implementing an acetylation reaction, after the reaction is completed, concentrating a reactionliquid, and separating an alpha-acetyl-gamma-butyrolactone sodium solid; implementing pulping and washing on the alpha-acetyl-gamma-butyrolactone sodium solid by using a second organic solvent in which the alpha-acetyl-gamma-butyrolactone sodium solid is not dissolvable; putting the washed alpha-acetyl-gamma-butyrolactone sodium solid into a third organic solvent, adjusting the pH value to 6-7 byusing an acid solution, stirring, filtering, and implementing vacuum distillation on filtrate, thereby obtaining alpha-acetyl-gamma-butyrolactone. The method has the characteristics of being short inpurification time, low in energy consumption, simple in preparation equipment, concise in operation, economically feasible, high in product purity, relatively high in yield, good in environment protection, and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical products, and in particular relates to a method for preparing α-acetyl-γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone is an important chemical product. There are two synthetic methods, 1. The process route using ethylene oxide and ethyl acetoacetate as starting materials, 2. Using γ-butyrolactone, Ethyl acetate is the process route of starting material. [0003] The ethylene oxide used in the first synthetic route is a first-class flammable and explosive chemical, and the reaction process is not easy to control, which is not conducive to production and storage, so it is not suitable for large-scale industrial production. The second synthetic route is to use γ-butyrolactone, and ethyl acetate is the synthetic route of starting raw material, and this route mainly is to make γ - Butyrolactone reacts with ethyl acetate to form α-acetyl-γ-butyrolactone. [00...

Claims

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Application Information

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IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 周宏白跃飞吴晓璟皮昌桥刘刈孙董军于河舟周凯胡勇南
Owner NORTHEAST PHARMA GRP
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