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High-pressure synthesis method of 2-phenylpropionic acid

A technology for phenylpropionic acid, high pressure synthesis, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve the problems of low production efficiency, large consumption of raw materials, slow reaction speed, etc., to improve production Efficiency, less raw material consumption, and faster reaction rate

Inactive Publication Date: 2019-06-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction speed is slow, the methylation and hydrolysis time is long, the production efficiency is low, and lye needs to be supplemented during the hydrolysis process, and the consumption of raw materials is large

Method used

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  • High-pressure synthesis method of 2-phenylpropionic acid
  • High-pressure synthesis method of 2-phenylpropionic acid
  • High-pressure synthesis method of 2-phenylpropionic acid

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0046] Example 1, a pressurized reaction-rectification device, such as figure 1 Said, including reactor B (column) with magnetic stirrer C and reaction temperature sensor T2, heating jacket D is set on the outer surface of reactor B, also includes rectifying column A, condenser E1, cooler E2, exhaust pressure control valve V1, pressure sensor P1, distillate temperature sensor T1;

[0047] The top outlet of reaction kettle B is connected with rectification tower A; the top outlet of rectification tower A is connected with cooler E2, and the fraction temperature sensor T1, pressure Sensor P1, exhaust pressure control valve V1; a condenser E1 is set between the side wall outlet near the top of the rectification tower A and the pressure sensor P1.

[0048] The heating jacket D is responsible for heating the reactor B, thereby controlling the reaction temperature in the reactor B; the reaction temperature sensor T2 is used to monitor the reaction temperature in the reactor B; the ...

Embodiment 1

[0050] Embodiment 1, a kind of method for synthesizing 2-phenylpropionic acid by autoclave method, carries out following steps successively:

[0051] Step 1), methylation reaction:

[0052]Add 15g (0.128mol) phenylacetonitrile, 7.5g (0.141mol) sodium methylate, 20.7g (0.23mol) dimethyl carbonate in the reaction kettle B of the pressurized reaction-rectification device, nitrogen leak detection and replacement, then heat up To 180°C (that is, T2 is 180°C), through the exhaust pressure control valve V1, control the top pressure of rectification tower A to 2Mpa (that is, P1 is 2MPa); the reaction time is 4h;

[0053] Gases emitted during the methylation reaction (including dimethyl carbonate, methanol, CO 2 ) enters the rectification tower A through the outlet at the top of the reactor B, and the top temperature of the rectification tower A is about 145°C (that is, T1 is 145°C); the methanol and carbon dioxide in the gas come out from the top of the rectification tower A , after...

Embodiment 2～9

[0063] Change the mol ratio of phenylacetonitrile, sodium methylate, dimethyl carbonate in step 1) in embodiment 1, conditions such as temperature of reaction, reaction time, all the other operations are equal to embodiment 1, obtain embodiment 2~9, concrete process parameter and The comparison between the results and Example 1 is shown in Table 1.

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PUM

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Abstract

The invention discloses a high-pressure synthesis method of 2-phenylpropionic acid. A pressurized reaction-rectification device is adopted, the method sequentially comprises the following steps: phenylacetonitrile, sodium alcoholate and dimethyl carbonate are added to a reactor B and heated to 160-200 DEG C for a methylation reaction; methanol and CO2 produced in the methylation reaction process are discharged out of the whole pressurized reaction-rectification device, after the methylation reaction ends, the reactor B is cooled for rectification under normal pressure, and dimethyl carbonate is obtained; after the reactor B is cooled to the room temperature, water is added to the reactor B, the temperature is increased to 120-180 DEG C for a hydrolysis reaction, after the hydrolysis reaction ends and the reactor B is cooled to the room temperature, acid is added to a reaction solution in the reactor B, the solution is left to stand for layering, and the upper layer is a crude product of 2-phenylpropionic acid. The method has the characteristics of high reaction rate, few three wastes, low production cost and the like when used for preparing 2-phenylpropionic acid.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for synthesizing 2-phenylpropionic acid by an autoclave method. Background technique [0002] 2-phenylpropionic acid, structural formula such as formula 1, it is one of the key intermediates of synthesizing loxoprofen sodium, loxoprofen sodium belongs to aryl propionic acid novel non-steroidal anti-inflammatory drug, has analgesic, anti-inflammatory It has anti-inflammatory and anti-rheumatic effects, and has important applications in medicine. [0003] [0004] At present, the industrial production of 2-phenylpropionic acid is mainly produced through methylation and hydrolysis of phenylacetonitrile. [0005] Patent CN105037139A mixes phenylacetonitrile, dimethyl carbonate, and sodium methoxide at a molar ratio of 1:5:2, then uses toluene as a solvent, raises the temperature to 20-100°C, controls the pressure at 0.5-6MPa, and reacts for 10 hours to recove...

Claims

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Application Information

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IPC IPC(8): C07C51/02C07C57/30C07C51/41C07C51/08C07C253/30C07C255/33
Inventor 陈新志曹忠钱超
Owner ZHEJIANG UNIV
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