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Preparation method of allyl amyl glycolate

A technology of Gapon ester and Gapon acid, which is applied in the preparation of carboxylate, the preparation of organic compounds, the preparation of carboxylate and other directions, can solve the problems of harsh reaction equipment and operation requirements, unfavorable industrial production and other problems, and achieves environmental protection without harm Efficiency, good market prospects, simple method effect

Inactive Publication Date: 2018-01-09
新乡市巨能合成材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The known synthesis process is to use sodium metal or sodium hydride and isoamyl alcohol as raw materials to first prepare sodium isoamyl alcohol, then react with chloroacetic acid dechlorinated sodium to generate isoamyloxyacetic acid, and the latter continues to react with propylene alcohol in In an acidic system, use a dehydrating agent to dehydrate to generate glycopyrrolate. This synthesis method will generate hydrogen gas by reacting with metal sodium. The reaction equipment and operation requirements are harsh, which is not conducive to industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) For the preparation of sodium chloroacetate, add 2700L isoamyl alcohol to the reaction kettle, then add 175Kg sodium hydroxide, heat up to 130°C and reflux for 3 hours, then control the temperature at 132-143°C to distill 1200L isoamyl alcohol, condense Cool down to 115°C and add 1200L of isoamyl alcohol evaporated from the above, continue to cool down to 80°C and add 1Kg alumina and 185Kg chloroacetic acid, stir and raise the temperature to 110°C and keep the temperature constant for 30min. 800L of isoamyl alcohol, after evaporation, cool down to 110°C, then add 1000L of water to the reaction kettle, stir evenly, then transfer the material, then add 300L water to wash the kettle, after washing, the transfer is completed, and finally the target product sodium chloroacetate is obtained. 98%, the product content is 96%;

[0016] (2) For the preparation of Geponic acid, heat the sodium chloroacetate obtained in step (1) to 98°C to reflux to remove isoamyl alcohol, keep...

Embodiment 2

[0019] (1) For the preparation of sodium chloroacetate, add 2500L isoamyl alcohol to the reaction kettle, then add 150Kg sodium hydroxide, heat up to 130°C and reflux for 3 hours, then control the temperature at 132-143°C to distill 1100L isoamyl alcohol, condense Cool down to 115°C and add 1100L of isoamyl alcohol evaporated from the above, continue to cool down to 80°C and add 0.5Kg alumina and 150Kg chloroacetic acid, stir to raise the temperature to 110°C and keep the temperature constant for 30min. Take out 800L isoamyl alcohol, cool down to 110°C after evaporating, then add 800L water to the reaction kettle, stir evenly, then transfer the material, then add 500L water to wash the kettle, after washing, the material transfer ends, and finally the target product sodium chloroacetate is obtained. The rate is 96%, and the product content is 96%;

[0020] (2) For the preparation of Geponic acid, heat the sodium chloroacetate obtained in step (1) to 98°C to reflux to remove is...

Embodiment 3

[0023] (1) For the preparation of sodium chloroacetate, add 3000L isoamyl alcohol to the reaction kettle, then add 200Kg sodium hydroxide, heat up to 130°C and reflux for 3 hours, then control the temperature at 132-143°C to distill 1300L isoamyl alcohol, condense Cool down to 115°C and add 1300L of isoamyl alcohol that was evaporated above, continue to cool down to 80°C, add 2Kg alumina and 200Kg chloroacetic acid, stir and raise the temperature to 110°C and keep the temperature constant for 30min. 800L of isoamyl alcohol, after evaporation, cool down to 110°C, then add 1200L of water to the reaction kettle, stir evenly, then transfer the material, then add 300L water to wash the kettle, after washing, the transfer is completed, and finally the target product sodium chloroacetate is obtained. 97%, the product content is 96%;

[0024] (2) For the preparation of Geponic acid, heat the sodium chloroacetate obtained in step (1) to 98°C to reflux to remove isoamyl alcohol, keep it...

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PUM

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Abstract

The invention discloses a preparation method of allyl amyl glycolate and belongs to the technical field of fine chemical engineering. The preparation method of the allyl amyl glycolate is characterized by specifically comprising the steps of preparing sodium chloroacetate, preparing galbanum acid, preparing the allyl amyl glycolate and the like. The allyl amyl glycolate is prepared by selecting ordinary industrial raw materials and adopting a simple preparation method. The method has the advantages of simplicity, environment friendliness, no hazards, relatively-high efficiency and a relatively-good market prospect.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of glycopyrrolate. Background technique [0002] At present, Ingoponate has a strong pineapple aroma, and is widely used in the flavoring of food, tobacco and daily chemicals. The chemical name of glycopyrrolate is: allyl isopentyloxyacetate. The known synthetic technique is to use sodium metal or sodium hydride and isoamyl alcohol as raw materials to first prepare sodium isoamyloxide, then react with chloroacetic acid dechlorinated sodium to generate isoamyloxyacetic acid, and the latter continues to react with propylene alcohol in In the acidic system, the dehydration agent is used to generate glycopyrrolate. This synthetic method reacts with metal sodium to generate hydrogen gas. The reaction equipment and operation requirements are harsh, which is not conducive to industrial production. Contents of the invention [0003] The technic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/708C07C67/08C07C51/41C07C53/16C07C51/367C07C51/02C07C59/125
Inventor 周忠太张学栋张全万张齐亮孟红文张小涛
Owner 新乡市巨能合成材料有限公司
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