Method for synthesizing phenylacetic acid from carbonyl

A technology of oxo synthesis and phenylacetic acid, applied in carbon monoxide reaction to prepare carboxylic acid, carboxylate preparation, organic chemistry, etc., can solve the problem of no industrialization report. In China, there are Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Sichuan University, Dalian University of Technology, etc. To achieve the effects of easy separation and treatment, easy recovery, and mild reaction conditions

Inactive Publication Date: 2019-03-08
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

In China, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Sichuan University, Dalian University of

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add a certain amount of cobalt chloride and methanol into the autoclave, replace it with CO gas for three times, slowly raise the temperature to 100~120℃ under stirring, and add CO gas to increase the internal pressure to 3.0~3.2MPa, continue After stirring, when the pressure in the kettle drops to 2.5MPa, ventilate to the original pressure again and continue until the internal pressure no longer drops. After maintaining for 8 hours, the pressure is released and the temperature is reduced to normal temperature. The suspension in the kettle is filtered, and the filter residue is used to recover cobalt. The filtrate is put into a storage tank and sealed with 0.2-0.3MPa CO to obtain a tetracarbonyl cobalt-methanol catalyst, which is metered out during the experiment.

[0036] In this embodiment, the molar ratio of catalyst to benzyl chloride is 0.02:1, and the molar ratio of benzyl chloride to NaOH is 0.25:1.

[0037] In a 1L reactor, replace with CO gas three times, add 3.04g ...

Embodiment 2

[0039] The methanol solution of cobalt tetracarbonyl in this example is the same batch of solution prepared in Example 1.

[0040] In this embodiment, the molar ratio of catalyst to benzyl chloride is 0.1:1, and the molar ratio of benzyl chloride to NaOH is 1:2.

[0041] In a 1L reactor, replace it with CO gas three times, add 17.56g of methanol solution containing cobalt tetracarbonyl, pass CO gas at a rate of 130mL / min, slowly increase the temperature to 65℃, keep the pressure at 0.1MPa, stir and start dripping Benzyl chloride and NaOH solution. The amount of benzyl chloride added was 130g, and the amount of NaOH solid was 82.2g. After the dropwise addition is completed, the reaction is continued for 4 hours, the temperature is lowered to room temperature, and air is introduced for 2 hours. The subsequent processing procedure is the same as in Example 1. 119.8 g of phenylacetic acid was obtained, the conversion rate of benzyl chloride was 99%, and the yield of phenylacetic aci...

Embodiment 3

[0043] The methanol solution of cobalt tetracarbonyl in this example is the same batch of solution prepared in Example 1.

[0044] In this embodiment, the molar ratio of catalyst to benzyl chloride is 0.05:1, and the molar ratio of benzyl chloride to NaOH is 1:2.

[0045] In a 1L reactor, replace with CO gas three times, add 8.78g of methanol solution containing cobalt tetracarbonyl, pass CO gas at a rate of 130mL / min, slowly increase the temperature to 90℃, keep the pressure at 0.5MPa, stir and start dripping Benzyl chloride and NaOH solution. The amount of benzyl chloride added was 130g, and the amount of NaOH solid was 82.2g. After the dropwise addition is completed, the reaction is continued for 8 hours, the temperature is lowered to room temperature, and air is introduced for 2 hours. The subsequent processing procedure is the same as in Example 1. 119.2 g of phenylacetic acid was obtained, the conversion rate of benzyl chloride was 99%, and the yield of phenylacetic acid w...

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Abstract

The invention provides a method for synthesizing phenylacetic acid from carbonyl, and belongs to the technical field of phenylacetic acid synthesis. According to the method, benzyl chloride, sodium hydroxide and CO are taken as raw materials, a tetracarbonyl cobalt-methanol solution is taken as a catalyst, sodium phenylacetate is generated through a carbonylation reaction at a certain temperatureand pressure, and then extraction, acidification, filtration and crystallization are performed to obtain a product, namely phenylacetic acid. According to the invention, the tetracarbonyl cobalt-methanol solution is taken as a catalyst, which has better activity and economy, and is more easily recovered than metal catalysts such as rhodium, platinum, iron, manganese and the like, and the cobalt recovery rate is up to 90% or more than 90%; the process provided by the invention is performed at low pressure and low temperature, the reaction conditions are mild, the material requirements on equipment are low, no poisons or odors are produced during the process, by-products generated are easy to be separated and treated, and the process is less in pollution and environmentally-friendly; the conversion rate of the raw materials is 99% or more than 99%; the yield of phenylacetic acid is 85% or more than 85%; and the purity of phenylacetic acid is 99.0% or more than 99.0%.

Description

Technical field [0001] The invention belongs to the technical field of phenylacetic acid synthesis, and is specifically a method for oxo synthesis of phenylacetic acid. Background technique [0002] Phenylacetic acid is an important chemical raw material and is widely used as an intermediate for medicines, pesticides and spices. At present, the main use of phenylacetic acid in China is for the production of penicillin. In the production process of penicillin, phenylacetic acid is added to increase the fermentation unit, and 0.8 tons of phenylacetic acid are needed to produce 1 ton of penicillin. [0003] There are many production methods of phenylacetic acid, and the industrialized production methods include sodium cyanide method, phenylacetamide method and oxo method. [0004] The sodium cyanide method (phenylacetonitrile hydrolysis method) takes toluene as a raw material, passes chlorine to generate benzyl chloride, reacts with sodium cyanide to generate benzyl chloride, and then ...

Claims

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Application Information

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IPC IPC(8): C07C51/10C07C51/02C07C57/32
CPCC07C51/02C07C51/10C07C57/32
Inventor 陈晓华贾绘如王莉谌晓玲周拥华鄢义
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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