Method for preparing acrivastine

A technology of avastatin and avastin, which is applied in the field of drug synthesis, can solve the problems of cumbersome operation steps, large amount of three wastes, and increased production costs, and achieve the effects of high purity, reduced operating hours, and low production costs

Inactive Publication Date: 2017-03-29
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above literature reports show that the treatment process after hydrolysis requires the use of organic solvents (such as methyl tert-butyl ether, isopropanol, methylene chloride, 1,4-dioxane, etc.) for extraction, washing, drying, and concentration Waiting for a series of operations, and then adding an organic solvent to crystallize for a long time, the operation steps are not only cumbersome, but the amount of three wastes to be treated is large, and the production cost is also increased

Method used

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  • Method for preparing acrivastine
  • Method for preparing acrivastine
  • Method for preparing acrivastine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a 100ml three-neck flask equipped with a stirrer and a thermometer, add 50g of anhydrous methanol, start stirring, then add 8.0g of ethyl arvalate, and protect with nitrogen. Heat up to 35°C-45°C to dissolve, then add 0.8g of activated carbon, keep warm for half an hour for decolorization. After filtering, the filtrate was transferred to a three-necked flask, and 26.5 g of 6.7% potassium hydroxide solution was added dropwise. Keeping the temperature at 35°C-45°C, after reacting for 1.0h, TLC spot plate (dichloromethane / methanol=9 / 1) showed that the reaction was complete. Concentrate under reduced pressure until the flow is cut off, add 8 g of purified water, cool down to 20°C-30°C, adjust the pH value to 5.0 with 6% sulfuric acid solution, stir for 10 minutes and repeat the test. Cool down to 5°C-15°C in an ice bath, and crystallize for 4 hours. Suction filtration, rinse the filter cake with purified water 8g×2, suction filtration, and dry the filter cake at 90°C u...

Embodiment 2

[0038]In a 100ml three-necked flask equipped with a stirrer and a thermometer, add 50g of absolute ethanol, start stirring, then add 8.0g of ethyl arvalate, and protect with nitrogen. Heat up to 35°C-45°C to dissolve, then add 2.0g of silica gel, keep warm for half an hour for decolorization. After filtering, the filtrate was transferred to a three-necked flask, and 28.4 g of 12% sodium carbonate solution was added dropwise. Raise the temperature to 60°C, react for 2 hours, TLC spot plate (dichloromethane / methanol=9 / 1) shows that the reaction is complete, concentrate under reduced pressure until the flow is cut off, add 16g of purified water, cool down to 20°C-30°C, and use 6% phosphoric acid The pH value of the solution was adjusted to 6.0, stirred for 10 minutes and retested. Cool down to 0°C-10°C in an ice bath, and crystallize for 3 hours. After suction filtration, the filter cake was rinsed with 16 g of purified water × 2, suction filtered, and the filter cake was dried...

Embodiment 3

[0040] In a 100ml three-necked flask equipped with a stirrer and a thermometer, add 50g of absolute ethanol, start stirring, then add 8g of ethyl avalate, and protect with nitrogen. Heat up to 35°C-45°C to dissolve, then add 0.8g of activated carbon, keep warm for half an hour for decolorization. After filtration, 26.5 g of 5% sodium hydroxide solution was added dropwise to the filtrate. Keeping the temperature at 35°C-45°C, after reacting for 1.0h, TLC spot plate (dichloromethane / methanol=9 / 1) showed that the reaction was complete. Concentrate under reduced pressure until the flow is cut off, add 8 g of purified water, cool down to 20°C-30°C, adjust the pH value to 6.5 with 6% sulfuric acid solution, stir for 10 minutes and repeat the test. Cool down to 0°C-10°C in an ice bath, and crystallize for 6 hours. After suction filtration, the filter cake was rinsed with purified water 8g×2, suction filtered, and the filter cake was dried under reduced pressure at 90°C to obtain 6....

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Abstract

The invention belongs to the field of pharmaceutical synthesis, and relates to a method for preparing acrivastine. The method comprises the steps of adopting an acriva ethyl ester compound as a raw material, dissolving the acriva ethyl ester compound into an organic solvent medium, adding an inorganic base for alkaline hydrolysis, and completing alkaline reaction to obtain a hydrolysate of the acriva ethyl ester compound; decompressing concentrating the hydrolysate of the acriva ethyl ester compound until stopping flowing, and obtaining a concentrate; and adding water into the obtained concentrate, cooling to be ranged from 20 DEG C to 30 DEG C, acidizing to enable pH (Potential of Hydrogen) to be ranged from 5.0 to 7.0, crystallizing through a temperature differential method, filtering and drying to obtain an acrivastine crude product. The method is simple to operate, low in cost, free of using an organic solvent, environmentally friendly and easy for industrial production, and the obtained acrivastine is high in yield, high in purity and stable in quality.

Description

technical field [0001] The invention belongs to the field of drug synthesis and relates to a method for preparing aclastine. Background technique [0002] Avastin is a compound shown in formula II, which is a phenazine antihistamine antiallergic drug launched by Glaxo Wellcome in the late 1980s. It is a derivative of Triprolidine, and its molecular formula is C 22 h 24 N 2 o 3 , the molecular weight is 348.444, the chemical name is (E,E)-3-[6-[1-(4-methylphenyl)-3-(1-pyrrolidinyl)-1-propenyl]-2-pyridine Base]-2-acrylic acid is a second-generation antihistamine drug with a pyrrolamine structure, and it is a highly competitive histamine H 1 Receptor antagonist, no obvious anticholinergic effect, low penetration ability to the central nervous system, has good curative effect on acute and chronic urticaria, allergic rhinitis and other allergic diseases, and can also relieve itching and hay fever . This product has no cardiotoxic reaction, and has mild drowsiness and occasi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/55
CPCC07D213/55
Inventor 谭涛邹华安李国扬
Owner CHONGQING HUABANGSHENGKAI PHARM
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