A kind of preparation method of 2-phenylpropionic acid

A technology of phenylpropionic acid and phenylpropionitrile, which is applied in the field of 2-phenylpropionic acid preparation, can solve the problems of complex production process equipment and high production cost, and achieve the effects of low production cost, simple equipment and high purity of finished products

Active Publication Date: 2018-04-17
ZHEJIANG BOJU NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above production process equipment is complicated and the production cost is high

Method used

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  • A kind of preparation method of 2-phenylpropionic acid
  • A kind of preparation method of 2-phenylpropionic acid
  • A kind of preparation method of 2-phenylpropionic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation method of 2-phenylpropionic acid in this embodiment includes the preparation stage of methyl 2-(phenylcyano)propionate, the preparation stage of 2-phenylpropionitrile and the stage of 2-phenylpropionic acid, and the specific steps are as follows:

[0029] 1) Preparation stage of methyl 2-(phenylcyano)propionate

[0030] Add phenylacetonitrile: dimethyl carbonate: toluene: sodium methoxide with a molar ratio of 1:1.5:10:1.05 into the drying reactor. Under stirring, the temperature is raised to 75°C and the temperature is kept for 5 hours; after the reaction, the pressure is normal. Distill the by-product methanol until no methanol is distilled out, cool to 35°C, add dimethyl sulfate DMS with a molar ratio of 1.0 dropwise at a temperature of 50°C, and keep the reaction at 50°C for 5 hours. Cool down to 35°C, add 1.0 part by weight of water, stir, dissolve, and separate into layers. Recover toluene by distillation under reduced pressure, and distill off toluene...

Embodiment 2

[0036] The preparation method of 2-phenylpropionic acid in this embodiment includes the preparation stage of methyl 2-(phenylcyano)propionate, the preparation stage of 2-phenylpropionitrile and the stage of 2-phenylpropionic acid, and the specific steps are as follows:

[0037] 1) Preparation stage of methyl 2-(phenylcyano)propionate

[0038] Add phenylacetonitrile: dimethyl carbonate: toluene: sodium methoxide with a molar ratio of 1:3:15:1.2 into the dry reaction kettle. Under stirring, the temperature is increased to 90°C, and the reaction is kept for 2 hours; after the reaction, the pressure is normal. Distill the by-product methanol until no methanol is distilled out, cool to 35°C, add dimethyl sulfate DMS with a molar ratio of 1.0 dropwise at a temperature of 75°C, and keep the reaction at 70°C for 2 hours. Cool down to 35°C, add 2.0 parts by weight of water, stir, dissolve, and separate into layers. Recover toluene by distillation under reduced pressure, and distill off tol...

Embodiment 3

[0044] The preparation method of 2-phenylpropionic acid in this embodiment includes the preparation stage of methyl 2-(phenylcyano)propionate, the preparation stage of 2-phenylpropionitrile and the stage of 2-phenylpropionic acid, and the specific steps are as follows:

[0045] 1) Preparation stage of methyl 2-(phenylcyano)propionate

[0046] Add phenylacetonitrile: dimethyl carbonate: toluene: sodium methoxide with a molar ratio of 1:5:30:2 into the dry reaction kettle. Under stirring, the temperature is raised to 60°C and the reaction is kept for 10 hours; after the reaction, the pressure is normal Distill the by-product methanol until no methanol is distilled out, cool to 35°C, add dimethyl sulfate (DMS) with a molar ratio of 1.5 at a constant speed at 90°C, and keep the reaction at 80°C for 1 hour. Cool down to 35°C, add 2.0 parts by weight of water, stir, dissolve, and separate into layers. Recover toluene by distillation under reduced pressure, and distill off toluene to obt...

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Abstract

The invention discloses a preparation method for 2-phenylpropionic acid. The preparation method is characterized by comprising a 2-phenyl-2-cyano methyl propionate preparation stage, a 2-phenyl propionitrile preparation stage and a 2-phenylpropionic acid preparation stage, wherein the 2-phenyl-2-cyano methyl propionate preparation stage comprises: mixing benzyl cyanide, dimethyl carbonate, methylbenzene and sodium methoxide to obtain a mixture, heating the mixture to 20-100 DEG C, controlling the pressure to 0.5-6MPa and carrying out thermal-insulation reaction for 1-10 hours; after the reaction is ended, steaming out a byproduct methanol under the normal pressure, cooling the mixture to 35 DEG C, dropwise adding dimethyl sulfate DMS at constant speed by controlling the temperature to 35-85 DEG C, and carrying out the thermal-insulation reaction for 1-10 hours at 45-105 DEG C after the dropwise-adding is ended; cooling to 35 DEG C, adding water, stirring, dissolving, and layering; desolventizing to recycle toluene, thereby obtaining compound ester; and carrying out basic hydrolysis reaction and acidification reaction to finally prepare a finished product, wherein the purity of the finished product is high, and the yield of the finished product is higher than 92%. Besides, the production process disclosed by the invention adopts simple equipment and is low in production cost.

Description

Technical field [0001] The invention relates to a method for preparing 2-phenylpropionic acid. Background technique [0002] At present, 2-phenylpropionic acid is one of the key intermediates for the synthesis of loxoprofen sodium. Loxoprofen sodium is a new type of arylpropionic acid non-steroidal anti-inflammatory drug. It is clinically shown that it is currently known Acid drugs have the best analgesic, anti-inflammatory, and anti-rheumatic effects, so they are favored by domestic and foreign experts and scholars, as well as by the medical community and patients. This product was developed and marketed by Japan's Sankyo Pharmaceutical Co., Ltd. in 1986, and is currently on the market in many countries including Japan, South Korea, Europe and the United States, and is growing strongly. [0003] The synthesis of 2-phenylpropionic acid disclosed in Chinese Patent 201110288939.9 is carried out in three steps. The reaction first takes styrene and a hydrochloric acid solution with a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/30C07C51/08
CPCC07C51/08C07C253/30C07C255/41C07C255/33C07C57/30
Inventor 龚华银周俊黄金慧周邦福
Owner ZHEJIANG BOJU NEW MATERIALS CO LTD
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