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Preparation method of glutaric acid

A technology of glutaric acid and cyclopentanol, applied in the field of chemical drug synthesis, can solve the problems of complicated process, operator and environmental hazards, etc., and achieves the effect of simple process flow, reduced operator and environmental hazards, and less pollution

Inactive Publication Date: 2020-01-03
黄焕军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that the existing glutaric acid synthesis method is cumbersome and has great harm to operators and the environment, and provides a glutaric acid preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Add 32g of potassium permanganate and 80g of cyclopentanol into a 250mL flask, add 10g of 40% dilute sulfuric acid solution dropwise through a constant pressure dropping funnel, stir and heat up to 50°C, and react for 30min, then add 4mol / L hydrochloric acid to adjust the pH to pH= 0.5, extracted three times with 100mL, 50mL, and 50mL ether respectively, then washed with water, combined the organic phases, distilled off ether and unreacted cyclopentanol under reduced pressure, raised the temperature to 150°C, and cooled to obtain glutaric acid.

Embodiment 2

[0011] Add 32g of potassium permanganate and 85g of cyclopentanol into a 250mL flask, add 9.8g of 40% dilute sulfuric acid solution dropwise through a constant pressure dropping funnel, stir and raise the temperature to 60°C, and react for 40min, then add 4mol / L hydrochloric acid to adjust the pH to pH =1, extracted three times with 100mL, 50mL, and 50mL ether respectively, washed with water, combined the organic phases, distilled under reduced pressure to remove ether and unreacted cyclopentanol, raised the temperature to 150°C, and cooled to obtain glutaric acid.

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PUM

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Abstract

The invention discloses a preparation method of glutaric acid. The method comprises the following steps: taking a potassium permanganate powder and cyclopentanol into a flask, then dropwise adding a 40% dilute sulfuric acid solution, performing stirring and heating to 45-70 DEG C, carrying out an oxidation reaction for a period of time, then adjusting pH to 0.5-1.5, adding diethyl ether to performextracting for three times, then performing washing with water twice, and distilling off diethyl ether and unreacted cyclopentanol in an organic phase to obtain glutaric acid. The method has the advantages of simple technological process, safety and environmental protection, and low toxicity, the harm to operators and the environment is greatly reduced, the cost is saved, and thereby the method has promotion value.

Description

technical field [0001] The invention relates to the technical field of chemical drug synthesis, in particular to a preparation method of glutaric acid. Background technique [0002] The traditional preparation method of glutaric acid is to heat γ-butyrolactone and potassium cyanide to 190-195°C, stir for 2 hours, cool down, add concentrated hydrochloric acid to acidify glutaric acid monoamide, and then hydrolyze to obtain glutaric acid acid, then heat and dissolve dihydropyran and 0.2N nitric acid in a boiling water bath, then cool in an ice-water bath, add concentrated nitric acid, dihydropyran is hydrolyzed and release nitrogen dioxide, when the temperature drops to 0°C, Add sodium nitrate, stir vigorously for 3 hours, stop cooling, raise the temperature to 25-30°C, evaporate under reduced pressure, and cool to obtain glutaric acid. This method is cumbersome, and potassium cyanide is a highly toxic compound, and the nitrogen dioxide generated during the preparation of glu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/31C07C55/12
CPCC07C51/31C07C55/12
Inventor 王存亮许灵艳严学文黄焕军王小桥
Owner 黄焕军