Process for preparing 3-amino-1-adamantanol

A kind of adamantanol and process technology, applied in the field of chemical synthesis preparation, can solve the problems of complicated operation and low yield

Inactive Publication Date: 2018-05-22
CHONGQING MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The problem to be solved by the present invention is to provide a new method for preparing 3-amino-1-adamantanol in order to overcome technical difficulties such as low yield and complex operation in the existing 3-ami

Method used

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  • Process for preparing 3-amino-1-adamantanol
  • Process for preparing 3-amino-1-adamantanol
  • Process for preparing 3-amino-1-adamantanol

Examples

Experimental program
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Effect test

Embodiment 1

[0032]Under ice-bath conditions, add 37.5ml of 98% concentrated sulfuric acid into the round bottom flask, add 3.75ml of 65% concentrated nitric acid under stirring, and continue stirring for 10min. When the temperature of the reaction solution dropped to 0°C, 3.75 g of amantadine hydrochloride was added in portions. After the addition was complete, the reaction was continued for 2 h in the ice bath, and then the ice bath was removed, and the reaction was continued for 2 h at room temperature. Transfer the system to a three-neck flask, add 60g of crushed ice while stirring, until the reaction solution turns clear dark green, put it in an ice bath, add an appropriate amount of potassium hydroxide solid, adjust the pH of the solution to > 12, and keep the solution on ice The reaction was continued for 1 h under bath conditions, producing a large amount of white sticky solid. Suction filtration, collect the filtrate, adjust the pH of the filtrate to 7-8 with concentrated hydrochl...

Embodiment 2

[0034] Under ice-bath conditions, add 75ml of 98% concentrated sulfuric acid to a 250ml three-necked flask with a thermometer, and then add 7.5ml of 65% concentrated nitric acid while stirring, and continue stirring for 10min. When the temperature of the reaction solution dropped to 5°C, 7.5 g of amantadine hydrochloride was added in portions, and after the addition was complete, the reaction was continued for 2 h in the ice bath, and then the ice bath was removed, and the reaction was continued for 2 h at room temperature. Transfer the system to a 500ml three-neck flask, add 120g of crushed ice while stirring, until the reaction solution turns clear dark green, put in an ice bath, add an appropriate amount of potassium hydroxide solid, adjust the pH of the solution to > 12, and keep The reaction was continued for 1 h under ice-bath conditions, and a large amount of white thick solid was produced. Suction filtration, collect the filtrate, adjust the pH of the filtrate to 7-8 w...

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Abstract

The invention discloses a process for preparing a vildagliptin intermediate 3-amino-1-adamantanol. According to the process, amantadine hydrochloride is taken as a starting raw material, and the 3-amino-1-adamantanol is obtained by carrying out a mixed acid reaction on H2SO4/HNO3, carrying out alkaline hydrolysis on KOH/H2O, and carrying out ethanol extraction. The process is characterized in thatseparation and purification can be performed by using an ethanol extraction process after the alkaline hydrolysis is finished, so that the product yield is greatly increased. The preparation processis easy in obtaining of raw materials, rapid in reaction and high in yield, thus being suitable for industrial production.

Description

technical field [0001] The invention relates to a process for preparing 3-amino-1-adamantanol, which belongs to the technical field of chemical synthesis preparation. Background technique [0002] Diabetes is a metabolic disease characterized by out-of-control chronic hyperglycemia caused by a variety of etiologies and accompanied by a variety of complications. In recent years, the incidence of diabetes has been increasing year by year. One of the major chronic diseases. As of 2015, there were more than 400 million diabetic patients worldwide, and it is estimated that by 2040, the number of diabetic patients worldwide will rise to 642 million. Diabetes has become a global public health problem. [0003] The pathogenesis of diabetes is mainly due to insufficient insulin secretion and (or) functional defects. Clinically, diabetes is mainly divided into type I diabetes and type II diabetes, and type II diabetes patients account for more than 90%. At present, the treatment of...

Claims

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Application Information

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IPC IPC(8): C07C213/00C07C215/44
CPCC07C213/00C07C215/44
Inventor 胡湘南廖琦张豪李毓飞甘润张明边煦霏
Owner CHONGQING MEDICAL UNIVERSITY
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