Preparation method for Arbidol intermediate

A technology of intermediates and preparation steps, which is applied in the field of preparation of Arbidol intermediates, can solve the problems of cumbersome operation, complex synthesis process, and low yield, and achieve the effects of simple process, high yield, and excellent product quality

Inactive Publication Date: 2018-08-03
NANAN CHUANGPEI ELECTRONICS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Technical problem to be solved by the present invention: Aiming at the complex synthetic process of Arb

Method used

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  • Preparation method for Arbidol intermediate
  • Preparation method for Arbidol intermediate
  • Preparation method for Arbidol intermediate

Examples

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Effect test

example 1

[0021] Weigh 5-methoxy-2-nitrophenol and ethyl acrylate at a molar ratio of 1:10, first put 5-methoxy-2-nitrophenol and ethyl acrylate into a three-necked flask, and then add The mass fraction is 30% acetic acid, the molar ratio of acetic acid and 5-methoxyl-2-nitrophenol is 4:1, the catalyst Pd / C of 5-methoxyl-2-nitrophenol mass 10%, successively Replace the gas in the three-necked flask with hydrogen and nitrogen for 2 times, exhaust the air in the bottle, and then pass hydrogen into the three-necked flask until the pressure in the three-necked flask is 0.3MPa, heat to 50°C, stir and react for 4 hours; recover after the reaction is completed Catalyst Pd / C, distill and recover excess ethyl acrylate, pour the reactants in the three-necked flask into cold water, filter with suction to obtain filter residue, wash and dry in an oven, and recrystallize after drying to obtain Arbidol Al intermediate, ethyl 5-methoxyindole-2-carboxylate.

example 2

[0023] Weigh 5-methoxy-2-nitrophenol and ethyl acrylate at a molar ratio of 1:13, first put 5-methoxy-2-nitrophenol and ethyl acrylate into a three-necked flask, and then add The mass fraction is 30% acetic acid, the molar ratio of acetic acid and 5-methoxyl-2-nitrophenol is 5:1, the catalyst Ru / C of 5-methoxyl-2-nitrophenol mass 13%, successively Replace the gas in the three-necked flask with hydrogen and nitrogen for 3 times, exhaust the air in the bottle, and then pass hydrogen into the three-necked flask until the pressure in the three-necked flask is 0.4MPa, heat to 55°C, stir and react for 5h; recover after the reaction is completed Catalyst Ru / C, distill and recover excess ethyl acrylate, pour the reactants in the three-necked flask into cold water, filter with suction to obtain filter residue, wash and dry in an oven, and recrystallize after drying to obtain Arbidol Al intermediate, ethyl 5-methoxyindole-2-carboxylate.

example 3

[0025] Weigh 5-methoxy-2-nitrophenol and ethyl acrylate at a molar ratio of 1:15, first put 5-methoxy-2-nitrophenol and ethyl acrylate into a three-necked flask, and then add Mass fraction is 30% acetic acid, the molar ratio of acetic acid and 5-methoxyl-2-nitrophenol is 6:1, the catalyst Raney nickel of 5-methoxyl-2-nitrophenol mass 15%, successively Replace the gas in the three-necked flask with hydrogen and nitrogen for 4 times, exhaust the air in the bottle, and then pass hydrogen into the three-necked flask until the pressure in the three-necked flask is 0.5MPa, heat to 60°C, stir and react for 6h; recover after the reaction is completed Catalyst Raney nickel, distill and recover excess ethyl acrylate, pour the reactants in the three-necked flask into cold water, filter with suction to obtain filter residue, wash and put it in an oven for drying, and recrystallize after drying to obtain Arbidol Al intermediate, ethyl 5-methoxyindole-2-carboxylate.

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Abstract

The invention belongs to the field of medical intermediates, and particularly relates to a preparation method for an Arbidol intermediate. 5-methoxy-2-nitrophenol and ethyl acrylate are taken as synthesis raw materials, noble metal catalyst is added, hydrogen is introduced, reaction temperature and reaction time are optimized, catalytic hydrogenation reduction reaction is carried out, and finally,ethyl 5-methoxyindole-2-carboxylate is prepared. In a reaction process, no organic solvents need to be added, a preparation technology is simplified, an obtained product is purer, a yield is higher,in addition, a technology is simple, and the preparation method has an important meaning in the research of the Arbidol intermediate.

Description

technical field [0001] The invention belongs to the field of pharmaceutical intermediates, in particular to a method for preparing an Arbidol intermediate. Background technique [0002] Arbidol is suitable for the prevention and treatment of adults and children with influenza A, influenza B, acute viral respiratory infections, and severe acute respiratory disease syndrome, including concurrent bronchitis and pneumonia. Early use of Arbidol hydrochloride after the onset of influenza can significantly shorten the duration of the disease, reduce the severity of symptoms, and improve cough, headache, fever, chills, sweating, sore throat, muscle aches and fatigue in influenza patients. Symptoms have obvious effects, and the safety is good, which is suitable for clinical promotion and use. [0003] Among them, ethyl 5-methoxyindole-2-carboxylate is the key intermediate for the preparation of Arbidol, therefore, the development of a raw material is cheap and easy to obtain, easy t...

Claims

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Application Information

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IPC IPC(8): C07D209/42
CPCC07D209/42
Inventor 王玉环
Owner NANAN CHUANGPEI ELECTRONICS TECH CO LTD
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