Preparation method for 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: 2015-11-11
ZHEJIANG BOJU NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above production process equipment

Method used

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  • Preparation method for 2-phenylpropionic acid
  • Preparation method for 2-phenylpropionic acid
  • Preparation method for 2-phenylpropionic acid

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0027] Example one:

[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. 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 reaction 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 to 35°C, add 1.0 part by weight of water, stir, dissolve, and separate into layers. Recover toluene by distillation under reduced pressure until no tolue...

Example Embodiment

[0035] Embodiment two:

[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. 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 raised to 90°C and the reaction is kept for 2 hours; after the reaction, the pressure Distill the by-product methanol until there is no methanol, then 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 until no toluene i...

Example Embodiment

[0043] Embodiment three:

[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. 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. The temperature is lowered to 35°C. Dimethyl sulfate (DMS) with a molar ratio of 1.5 is added dropwise at a temperature of 90°C at a constant rate, and the reaction is kept 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 t...

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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 preparation method of 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 belongs to the aryl propionic acid class of new non-steroidal anti-inflammatory drugs. The analgesic, anti-inflammatory and anti-rheumatic effects of acid drugs are the best, so they are favored by experts and scholars at home and abroad, as well as respected by the medical profession and patients. This product was developed and launched by Sankyo Pharmaceutical Co., Ltd. in Japan in 1986. It has been launched in Japan, South Korea, Europe, America and many other countries, with a strong growth momentum. [0003] The synthesis of 2-phenylpropionic acid disclosed in Chinese patent 201110288939.9 is carried out in three steps. The reaction first uses styrene and a hydrochloric acid solution with a mass concentration of 20-25% as ...

Claims

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Application Information

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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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