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A kind of 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 problems such as high energy consumption, pollution, hidden dangers, etc., and achieves increasing feeding amount, reducing environmental pollution and eliminating pollution Effect

Active Publication Date: 2011-12-07
鞠彩霞
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN 101092407A discloses a method for continuously feeding gasified γ-butyrolactone and ethyl acetate into a fixed-bed reactor equipped with a supported solid alkali fluoride catalyst for reaction, but the production process , the energy consumption is large, and at the same time, using solid alkali fluoride as a catalyst has certain hidden dangers to products and environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The acetylating agent used in this embodiment is ethyl acetate. The acylation reactor (5L) was evacuated, then purged with nitrogen, then 1232g of γ-butyrolactone, 1894g of ethyl acetate and 100g of sodium metal were added, stirring was started, and the temperature was raised. After the system was refluxed, the nitrogen flow was stopped. Under the reflux state of the system, 280g of sodium metal was added continuously, and the speed of adding sodium metal was advisable to keep the reaction system stable. After the addition, continue the insulation reaction for 8h. Cool down to 30°C, gradually add about 2930g of 51% phosphoric acid solution under stirring, and neutralize until the pH of the system is between 3-4. After the neutralization, the layers were separated, the organic phase was separated, the aqueous phase was extracted once with 433g of toluene, and the organic phases were combined. Then first normal pressure (71 DEG C-90 DEG C) distills out the light compone...

Embodiment 2

[0021] The acetylating agent used in this embodiment is methyl acetate. Except that the acetylating agent uses 1595g methyl acetate to replace 1894g ethyl acetate in Example 1, all the other steps are the same as in Example 1. 1663.6 g of the product was obtained, the product purity was greater than 99.2%, and the yield reached 90.0%. The extracted aqueous phase was dehydrated to obtain 1878 grams of phosphate.

Embodiment 3

[0023] The acetylating agent used in this embodiment is a mixed ester of ethyl acetate and methyl acetate. Except that acetylating agent uses 947g ethyl acetate and 797g methyl acetate to replace 1894g ethyl acetate in embodiment 1, all the other steps are all the same as embodiment 1. 1674.5 g of the product was obtained, the product purity was greater than 99.1%, and the yield reached 90.5%. The extracted aqueous phase was dehydrated to obtain 1875 grams of phosphate.

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Abstract

The invention provides a method for preparing α-acetyl-γ-butyrolactone, which uses γ-butyrolactone and an acetylating agent (ethyl acetate, methyl acetate or a mixture of the two) as starting materials, Sodium metal is used as a catalyst, and the product is obtained through acylation, neutralization and distillation. The advantages of the present invention are: raw materials are used as solvent in the initial stage of acylation reaction, which reduces the environmental pollution caused by the solvent, increases the feeding amount, improves the production efficiency, and reduces the production cost; metal sodium is added into the reaction system in stages or continuously, effectively It avoids safety hazards such as punching and burning caused by the reaction at the melting temperature of metallic sodium, which causes the reaction speed to be difficult to control; by adopting the method of pressure-regulated distillation, the by-products are effectively recovered, reducing environmental pollution and improving comprehensive economic benefits.

Description

technical field [0001] The invention relates to medicine and chemical intermediates, in particular to a preparation method of α-acetyl-γ-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone is an important drug and organic chemical intermediate or raw material, especially as an intermediate for the production of vitamin B1, chloroquine and other drugs. At present, there are mainly two routes for the preparation of α-acetyl-γ-butyrolactone. One is a process using ethylene oxide and ethyl acetoacetate as starting materials, and the other is a process based on γ-butyrolactone. And ethyl acetate as the starting material process. [0003] US 2443827, CN 135745A, GB 740993, Czechoslovakia patent 95116, special agent Zhao 4212662 bulletin all adopt the synthesis process using ethylene oxide as raw material, but the ethylene oxide as the reaction raw material belongs to the first class flammable and explosive chemical There are serious safety hazards in storage, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33
Inventor 张生万王伟吴菊花祁成福付晋平胡永钢李美萍冯彦琳
Owner 鞠彩霞
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