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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 failure to realize the organic solvent-free process, sodium addition device and control system, and improve the comprehensive Economic benefits, inhibition of side reactions, and high yield

Active Publication Date: 2011-04-27
寿阳县世纪精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the reaction process, metal sodium is added in batches or continuously, and the requirements for the sodium addition device and control system are high. In addition, the water phase still needs to be extracted with solvent toluene after acidification, and a complete organic solvent-free process cannot be realized.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a fully dried acylation reaction kettle (50L) equipped with an electric stirrer, a condenser, and a thermometer, add 11.67kg of γ-butyrolactone and 17.90kg of ethyl acetate, start stirring, and add a mixture with a specific surface area of ​​1.1 at room temperature. cm 2 3.43kg of sodium metal per gram, then slowly heat up, and when the system is refluxed, stop heating. At this time, the temperature of the system rose to the highest temperature of 88° C. during the acylation process, and then the temperature of the system gradually decreased until it dropped to 75° C., then heating was started, and the reaction was maintained at reflux temperature for 12 hours. After the heat preservation is completed, the reaction solution is transferred to the neutralization kettle, and absolute ethanol and excess ethyl acetate are steamed out under normal pressure; then the temperature is lowered, and when the temperature is down to 58° C., 26.95 kg of 51% phosphoric acid solution...

Embodiment 2

[0020] In a fully dried acylation reaction kettle (50L) equipped with an electric stirrer, a condenser, and a thermometer, add 12.32kg of γ-butyrolactone and 15.92kg of methyl acetate, start stirring, and add at room temperature cm 2 / g of 3.6kg sodium metal, then slowly heat up, and when the system is refluxed, stop heating. At this time, the temperature of the system rose to the highest temperature of 83° C. during the acylation process, and then the temperature of the system gradually decreased until it dropped to 75° C., then heating was started, and the reaction was maintained at reflux temperature for 12 hours. After the heat preservation is finished, the reaction solution is transferred to the neutralization kettle, and anhydrous methanol and excess methyl acetate are steamed out under normal pressure; then the temperature is lowered, and when the temperature is down to 56° C., 28.5 kg of 51% phosphoric acid solution (this When the pH of the system is 3~4), after the a...

Embodiment 3

[0022] In the fully dried acylation reactor (50L) with an electric stirrer, condenser, and thermometer, add 12.32kg of γ-butyrolactone, 9.47kg of ethyl acetate and 7.97kg of methyl acetate, start stirring, and The lower specific surface area is 1.15cm 2 / g of 3.6kg sodium metal, then slowly heat up, and after the system is refluxed, stop heating. At this time, the temperature of the system rose to the highest temperature of 86° C. during the acylation process, and then the temperature of the system gradually decreased until it dropped to 75° C., then heating was started, and the reaction was maintained at reflux temperature for 12 hours. After the heat preservation is completed, the reaction solution is transferred to a neutralization kettle, and absolute ethanol, absolute methanol, excess ethyl acetate and methyl acetate are evaporated under normal pressure; then the temperature is lowered, and when the temperature drops to 60°C, gradually add 51 % phosphoric acid solution 2...

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PUM

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Abstract

The invention provides a preparation method of an alpha-acetyl-gamma-butyrolactone. The method comprises the following steps: firstly, adding gamma-butyrolactone, an acetylating agent and a catalyst which are used as raw materials into an acylating kettle which is fully dried under the condition of stirring; and then, slowly heating, acylating, neutralizing and rectifying to obtain a product. The invention has the advantages that before reaction, all materials are added into the acylating kettle which is fully dried in advance, then the materials are slowly heated and acylated, and the acylating kettle has no need of vacuum pumping and nitrogen purging, thus the invention is simple and convenient in operation and is easy to realize industrialized production; by controlling the specific surface area of sodium metal and carrying out the acylation reaction under the mild condition that the temperature is lower than 90DEG C, serious potential safety hazards such as blanking, combustion, explosion and the like are completely eradicated, the occurrence of the side reaction is inhibited, the product has high purity and yield, and the by-product is simple in composition and can be recovered easily; and organic solvents are not used in the whole production process, thereby fundamentally eliminating the pollution source, and greatly lowering the production cost.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical intermediates and chemical raw materials, in particular to a preparation method of α-acetyl-γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone is an important pharmaceutical intermediate and organic chemical raw material. 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 a process based on γ-butyrolactone. Processes starting with lactones and acetates. [0003] The synthesis process uses ethylene oxide as a raw material. The raw material ethylene oxide is a first-class flammable and explosive chemical, and there are serious unsafe hazards in the storage, transportation and reaction process. [0004] The synthesis process using γ-butyrolactone and acetate as starting materials is generally in toluene solvent, adding catalyst me...

Claims

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Application Information

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IPC IPC(8): C07D307/33B01J23/04
Inventor 张生万王伟祁成福付晋平李美萍赵振华陈雪敏胡永钢冯彦琳
Owner 寿阳县世纪精细化工有限公司
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