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Method for preparing phenylacetic acid by non-catalyzed hydrolysis of benzene acetonitrile in near-critical water medium

A near-critical water, catalytic hydrolysis technology, applied in the field of carboxylic acids, can solve the problems of complex process flow, imperfect catalyst preparation, selection and recovery, etc., achieve simple reaction process, high product purity and yield, and improve yield Effect

Inactive Publication Date: 2008-04-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process is complicated, and the preparation, selection and recovery of catalysts are not yet perfect

Method used

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  • Method for preparing phenylacetic acid by non-catalyzed hydrolysis of benzene acetonitrile in near-critical water medium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 340g of deionized water and 170g of phenylacetonitrile (the mass ratio of deionized water to phenylacetonitrile is 2:1) in a 500mL intermittent autoclave, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 5min, and use water Remove the air in the kettle by steam; close the exhaust valve, and continue to heat up to 240 ° C for 8 hours; the reaction product is cooled and crystallized to obtain crude phenylacetic acid. The crude product of phenylacetic acid was decolorized by activated carbon, recrystallized and dried in vacuum to obtain 139.1 g of phenylacetic acid product, the product was analyzed by HPLC with a purity of 98.4% (wt%) and a yield of 81.8%.

Embodiment 2

[0025] Add 360g of deionized water and 120g of phenylacetonitrile (the mass ratio of deionized water to phenylacetonitrile is 3:1) into a 500mL intermittent autoclave, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 2min, and use water Remove the air in the kettle by steam; close the exhaust valve, and continue to heat up to 250°C for 7 hours; the reaction product is cooled and crystallized to obtain a crude product of phenylacetic acid, which is decolorized with activated carbon, recrystallized, and vacuum-dried to obtain 96.96g of phenylacetic acid product, which is tested by HPLC The analytical purity was 98.7% (wt%) and the yield was 80.8%.

Embodiment 3

[0027] Add 360g of deionized water and 60g of phenylacetonitrile (the mass ratio of deionized water to phenylacetonitrile is 6:1) into a 500mL intermittent autoclave, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 4min, and use water Remove the air in the kettle by steam; close the exhaust valve, and continue to heat up to 250°C for 7 hours; the reaction product is cooled and crystallized to obtain a crude product of phenylacetic acid. The crude product is decolorized with activated carbon, recrystallized, and vacuum-dried to obtain 45.96g of phenylacetic acid product. The product is tested by HPLC The analytical purity was 99.1% (wt%) and the yield was 76.6%.

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Abstract

The present invention discloses a no-catalysis hydrolysis preparation method of benzeneacetic acid with benzyl cyanide in critical water mediator. The method includes the following procedures that: firstly deionized water and benzyl cyanide are added into a high-pressure reactor with the mass ratio of 2:1-8:1, the mixture is agitated openly and the temperature is raised up to boiling point under the normal pressure, then the exhaust valve is kept open for 2-5 minutes; secondly the exhaust valve is kept closed, and the temperature is continuously raised up to 240 DEG C to 310 DEG C for hydrolysis for 1-8 hours; thirdly the hydrolysate is cooled down and crystallized, and crude benzeneacetic acid is obtained; fourthly the crude benzeneacetic acid is decolored with active carbon, secondarily crystallized and dried in vacuum to obtain the product of benzeneacetic acid. The present invention has no need to add any catalyst during the reaction process, thereby solving the puzzle of pollution of catalyzed hydrolyzation of acid and alkali, and having the advantages of simple process, green operation, high purity and high yield.

Description

technical field [0001] The invention relates to carboxylic acids, in particular to a method for preparing phenylacetic acid by non-catalytic hydrolysis of phenylacetonitrile in a near-critical water medium. Background technique [0002] Phenylacetic acid (CAS No: 103-82-2), also known as phenylacetic acid, has a molecular formula of C8H8O2 and a structural formula of: ), flaky white crystals with plant aroma. Phenylacetic acid is a component of many plants and is commonly found in high boiling fractions of neroli and peppermint oils. [0003] Phenylacetic acid can undergo a typical reaction of carboxyl, methylene hydrogen and benzene ring to generate many useful intermediates. It is an important organic chemical raw material and has a wide range of uses in medicine, industry and agriculture. In the pharmaceutical industry, phenylacetic acid is the precursor for the fermentation of penicillin, and is also used in the preparation of sedative, antidepressant (amitriptyline) ...

Claims

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Application Information

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IPC IPC(8): C07C57/32C07C51/08
Inventor 吕秀阳石超君
Owner ZHEJIANG UNIV
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