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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

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

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation method of the present embodiment 2-phenylpropionic acid comprises the preparation stage of 2-(phenylcyano)methyl 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 in a molar ratio of 1: 1.5: 10: 1.05 into the dry reaction kettle, heat up to 75°C under stirring, and keep warm for 5 hours; Evaporate the by-product methanol until no methanol is evaporated, lower the temperature to 35°C, and add dimethyl sulfate DMS with a molar ratio of 1.0 dropwise at a constant speed at a temperature of 50°C, and keep the reaction at 50°C for 5 hours after dropping. Cool down to 35°C, add 1.0 parts by weight of water, stir, dissolve, and separate layers. Toluene is recovered by distillation under reduced pressure until no toluene is evaporat...

Embodiment 2

[0036] The preparation method of the present embodiment 2-phenylpropionic acid comprises the preparation stage of 2-(phenylcyano)methyl 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 in a molar ratio of 1:3:15:1.2 into the dry reaction kettle, heat up to 90°C under stirring, and keep warm for 2 hours; Evaporate by-product methanol until no methanol is evaporated, lower the temperature to 35°C, and add dimethyl sulfate DMS with a molar ratio of 1.0 dropwise at a constant speed at a temperature of 75°C, and keep the reaction at 70°C for 2 hours after dropping. Cool down to 35°C, add 2.0 parts by weight of water, stir, dissolve, and separate layers. Toluene is recovered by distillation under reduced pressure until no toluene is evaporated to obta...

Embodiment 3

[0044] The preparation method of the present embodiment 2-phenylpropionic acid comprises the preparation stage of 2-(phenylcyano)methyl 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 in a molar ratio of 1:5:30:2 into the dry reaction kettle, heat up to 60°C under stirring, and keep warm for 10 hours; The by-product methanol was distilled until no methanol was distilled out, the temperature was lowered to 35°C, the temperature was controlled at 90°C, and dimethyl sulfate (DMS) with a molar ratio of 1.5 was added dropwise at a constant speed, and the reaction was kept at 80°C for 1 hour after dropping. Cool down to 35°C, add 2.0 parts by weight of water, stir, dissolve, and separate layers. Toluene is recovered by distillation under reduced pres...

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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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