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Preparation method and post-treatment process of 4-aminopyridine

An aminopyridine and process technology, which is applied in the field of chemical raw material synthesis, can solve the problems of high requirements on reaction conditions, high catalyst costs, and low yields, and achieve the effects of mild reaction conditions, easy control, simple post-treatment methods, and simple operations

Active Publication Date: 2020-05-12
山东泓达生物科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Comparing the preparation method and post-treatment process of the above-mentioned 4-aminopyridine, it is not difficult to find that: the preparation of the above 4-aminopyridine mostly needs to add a catalyst, and the cost of the catalyst is relatively high. Difficult to recycle, especially the post-treatment process requires continuous extraction of organic solvents for tens of hours or multiple extractions, which greatly increases the production cost. These disclosed methods for the preparation of aminopyridines all have high requirements for reaction conditions, more pollution from three wastes, and require more One-step reaction leads to problems such as low yield, which is not suitable for industrial production application

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  • Preparation method and post-treatment process of 4-aminopyridine

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Embodiment 1

[0031] A preparation method and post-treatment process of 4-aminopyridine, the steps of which are:

[0032] S1: Using isonicotine as a raw material, carry out Hoffman degradation reaction in sodium hypochlorite solution and 10% sodium hydroxide solution; first pour 195g of sodium hypochlorite solution into a four-necked flask (wherein the sodium hypochlorite solution has an available chlorine content of 6 %), the four-neck flask was placed in a 0°C cold trap to cool down while stirring was started. When the temperature of the sodium hypochlorite solution in the four-necked flask drops below 10°C, 20 g of solid isonicotine is added at this time, and after stirring until clarification, the stirring reaction is continued. Test the pH value and use HPLC to detect whether the isonicotine is completely converted into an intermediate, then add 10g of 10% sodium hydroxide solution to adjust the feed liquid to strong alkalinity, then transfer it to a water bath to slowly heat up, keep ...

Embodiment 6

[0039] A preparation method and post-treatment process of 4-aminopyridine, the steps of which are:

[0040] S1: Using isonicotine as raw material, carry out Hoffmann degradation reaction in sodium hypochlorite solution and 10% sodium hydroxide solution; first, pour 580g of sodium hypochlorite solution into a four-necked flask (among them, the sodium hypochlorite solution has an available chlorine content of 7.5 %), the four-neck flask was placed in a 0°C cold trap to cool down while stirring was started. After the temperature of the sodium hypochlorite solution in the four-neck flask dropped below 10°C, 75 g of solid isonicotine was added at this time, and after stirring until clarified, the stirring reaction was continued. Test the pH value and use HPLC to detect whether the isonicotine is completely converted into an intermediate, then add 30g of 10% sodium hydroxide solution to adjust the feed liquid to strong alkalinity, then transfer it to a water bath to slowly heat up, ...

Embodiment 8

[0047]S1: Using isonicotine as a raw material, carry out Hoffmann degradation reaction in sodium hypochlorite solution and 10% sodium hydroxide solution; first pour 365g of sodium hypochlorite solution into a four-necked flask (wherein the sodium hypochlorite solution has an available chlorine content of 12 %), the four-neck flask was placed in a 0°C cold trap to cool down while stirring was started. After the temperature of the sodium hypochlorite solution in the four-neck flask dropped below 10°C, 75 g of solid isonicotine was added at this time, and after stirring until clarified, the stirring reaction was continued. Test the pH value and use HPLC to detect whether isonicotine is completely converted into an intermediate, then add 19g of 10% sodium hydroxide solution to adjust the feed liquid to strong alkalinity, then transfer it to a water bath to slowly heat up, keep warm for a certain period of time, and set a certain time during the reaction. Samples were taken for HPL...

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Abstract

The invention relates to a preparation method and a post-treatment process of 4-aminopyridine. The preparation method comprises the following steps: with isonicotine as an initial raw material, carrying out a Hofmann degradation reaction in a sodium hypochlorite solution and a sodium hydroxide solution, carrying out cooling treatment on a reaction solution, and then successively performing activated carbon decoloration, cooling crystallization, vacuum filtration and drying, and secondary recrystallization and drying to obtain a final 4-aminopyridine product. The whole reaction conditions are mild and easy to control, the operation is simple, the purity of the 4-aminopyridine reaches 99% or above, and the post-treatment process is simple, convenient and easy to operate, has a total yield of90% or above and is a post-treatment technology suitable for industrial production and application.

Description

technical field [0001] The invention relates to the field of synthesis of chemical raw materials, in particular to a preparation method and post-treatment process of 4-aminopyridine. Background technique [0002] Aminopyridine is an important class of derivatives of pyridine, which is widely used in the field of chemical engineering. With the continuous development and progress of science and technology, the application range of aminopyridine compounds is showing an upward trend year by year. Among them, 4-aminopyridine, as one of the aminopyridine compounds, is mainly used in the synthesis of dyes, pesticides and pharmaceutical intermediates, and is also used as a chemical reagent. The method for preparing 4-aminopyridine mainly contains the following several technological routes: one is synthesized by halopyridine compound catalytically; the other is synthesized by catalytic hydrogenation of nitropyridine; ; The fourth is synthesized by electrochemical methods; the fifth...

Claims

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Application Information

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IPC IPC(8): C07D213/73
CPCC07D213/73Y02P20/584
Inventor 宋彩玲卢魁明刘天琪陈加良刘伟
Owner 山东泓达生物科技有限公司
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