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Continuous production method and device of amantadine

A technology of amantadine and its production method, which is applied in the field of continuous production method and device of amantadine, which can solve the problems of enlarged production feeding and loading, large equipment and site occupation, high safety risk, etc., and achieve high production efficiency and equipment And the effect of less space occupation and high safety

Pending Publication Date: 2022-04-29
ZHEJIANG APELOA KANGYU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the deficiencies of the existing industrial production technology, the present invention independently designs and improves the high-viscosity reactor according to the characteristics of the amination process, and adopts the improved high-viscosity reactor to provide a continuous production method of amantadine, which can effectively solve the current There are problems such as low yield and low purity in the amination process, small feeding and loading capacity in scale-up production, large equipment and site occupation, low production efficiency, and high safety risks.

Method used

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  • Continuous production method and device of amantadine
  • Continuous production method and device of amantadine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1kg of 1-bromoJingang Dai alkane and 450g of urea were added into a premixer and mixed evenly. Heat the high-viscosity reactor to 240-250℃, open the vent of the secondary sublimation material condensation bin, start the stirring, set the rotation speed at 65 rpm, then start the feed screw to continuously add the premixed materials into the high-viscosity reactor, control the feed speed at 90-100 g / min, and react at the reactor temperature of 240-250℃ for 25-30 minutes. The materials in the reactor melt first, and then gradually change from liquid to solid. Adding water into the crude product, filtering, adding dichloromethane into the filtrate for extraction and layering, adding liquid alkali into the upper water phase for alkalization, filtering and drying to obtain amantadine product 660.2g with a yield of 93.9% and a GC purity of 98.68%.

Embodiment 2

[0048] 1kg of 1-bromoJingang Dai alkane and 335g of urea were added into a premixer and mixed evenly. Heat the high-viscosity reactor to 200-220℃, open the vent of the secondary sublimation material condensation bin, start the stirring, set the rotation speed at 50 rpm, then start the feed screw to continuously add the premixed materials into the high-viscosity reactor, control the feed speed at 45-55g / min, and react at the reactor temperature of 200-220℃ for 50-60 minutes. The materials in the reactor melt first, and then gradually change from liquid to solid. Adding water into the crude product, filtering, adding dichloromethane into the filtrate for extraction and layering, adding liquid alkali into the upper water phase for alkalization, filtering and drying to obtain amantadine product 638.4g with a yield of 90.8% and a GC purity of 97.97%.

Embodiment 3

[0050] 1kg of 1-bromoJingang Dai alkane and 558g of urea were added into a premixer and mixed evenly. Heat the high-viscosity reactor to 280 ~ 300℃, open the vent of the secondary sublimation material condensation bin, start stirring, set the rotation speed to 80 rpm, then start the feed screw to continuously add the premixed material into the high-viscosity reactor, control the feed speed to 100 ~ 110 g / min, and react at the reactor temperature of 280 ~ 300℃ for 20 ~ 25 minutes. The material in the reactor melts first, then gradually changes from liquid to liquid. Adding water into the crude product, filtering, adding dichloromethane into the filtrate for extraction and layering, adding liquid alkali into the upper water phase for alkalization, filtering and drying to obtain amantadine product 648.9g with a yield of 92.3% and a GC purity of 98.48%.

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Abstract

The invention discloses a continuous production method and device of amantadine, and the method is as follows: uniformly mixed raw materials are continuously fed into a high-viscosity reactor preheated to a certain temperature, the materials rotate along with a stirring shaft in the high-viscosity reactor and move to a discharge port along the stirring shaft, and gas generated in the reaction process is discharged through a secondary sublimation material condensation bin; the first-stage condensed material is automatically cleaned and returned to the reactor, the second-stage condensed material is collected and purified to obtain adamantanol, the reacted material is continuously discharged from a discharge port of the reactor, an amantadine crude product is obtained through collection, and the amantadine crude product is treated to obtain an amantadine product. The method is simple to operate, high in product yield and purity, short in reaction time, high in production efficiency and small in equipment and site occupation, the collected and purified adamantanol can be sold, the mass and heat transfer effect of the reaction is enhanced by adopting the high-viscosity reactor, the safety risk caused by rapid heating and rapid gas production in the intermittent amination reaction process is avoided, and the method is suitable for industrial production. And the method is a continuous industrial production process with high safety.

Description

Technical field [0001] The invention belongs to the technical field of chemical pharmacy, and relates to a continuous production method and device of amantadine. technical background [0002] Amantadine is a symmetrical tricyclic amine, which is the earliest antiviral drug used to inhibit influenza virus. It can inhibit virus from penetrating into host cells, affect virus shelling, inhibit virus reproduction, prevent and treat cold caused by virus infection, and relieve and treat Parkinson's syndrome, various kinds of paralysis agitans, chronic hepatitis C, dementia and other diseases. [0003] There are many reports on the synthesis of amantadine, mainly focusing on the synthesis of amantadine and its hydrochloride from amantadine. Among them, it is the current industrial production route to take amantadine as the starting material and react with bromine to form 1- bromoJingang Dai alkane, and then react with urea to obtain amantadine. [0004] [0005] In this route, adamanta...

Claims

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Application Information

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IPC IPC(8): C07C209/08C07C209/84C07C211/38B01J19/00
CPCC07C209/08C07C209/84B01J19/0053B01J19/0046B01J19/0013C07C2603/74C07C211/38
Inventor 徐新良杨张艳庄程翰庄江海唐武期张伟金健笑陈奔祥
Owner ZHEJIANG APELOA KANGYU PHARMA
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