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Synthesis process of 3-aminopyridine

A synthesis process and aminopyridine technology, applied in the field of synthesis technology of 3-aminopyridine, can solve the problems of high cost, troublesome waste water treatment, unsuitable for industrial mass production and application, etc., and achieve high yield, simple preparation steps, high yield effect

Pending Publication Date: 2022-05-06
陕西菲尔特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the above-mentioned related technologies have the following defects: most of these reactions need to use metal catalysts, the cost is high, and the waste water treatment is troublesome, so they are not suitable for industrial mass production applications

Method used

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  • Synthesis process of 3-aminopyridine
  • Synthesis process of 3-aminopyridine
  • Synthesis process of 3-aminopyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The synthetic technique of 3-aminopyridine comprises the following synthetic steps:

[0034] Step 1: Preparation of nicotinamide: The device for nicotinamide preparation uses a reflux device, specifically adding 60ml of water to a three-necked beaker, and then adding 12.5g of 3-cyanopyridine and 1g of anhydrous sodium carbonate in sequence, stirring while reacting, and Slowly heat up to 73°C, and then keep warm for about 6 hours until the end of the reaction. After reaching the end of the reaction, cool to room temperature and stop stirring to obtain a reaction solution containing nicotinamide for later use.

[0035] During the preparation of nicotinamide, when determining the end point of the reaction, high-performance liquid chromatography is used for detection. The chromatographic conditions are as follows: chromatographic column: C18, 300mm*3.9mm, 5μm; detection wavelength: 254nm; mobile phase: methanol: 0.005mol / L sodium heptanesulfonate=30:70; flow rate: 1ml / min....

Embodiment 2

[0043] The synthetic technique of 3-aminopyridine comprises the following synthetic steps:

[0044] Step 1: Preparation of nicotinamide: The device for nicotinamide preparation uses a reflux device. Add 60ml of water into a three-necked beaker, then add 12.5g of 3-aminopyridine and 1g of anhydrous sodium carbonate in sequence, stir while reacting, and slowly heat up to 75°C, and then keep warm for about 6 hours until the end of the reaction. After reaching the end of the reaction, cool to room temperature, stop stirring, and obtain a reaction solution containing nicotinamide for later use.

[0045] The judgment of the reaction end point during the preparation of nicotinamide is the same as in Example 1;

[0046] Step 2: Add the nicotinamide-containing reaction liquid in step 1 into the sodium hydroxide solution, and keep the temperature at 2°C during the addition; then add the sodium hypochlorite solution and stir to obtain the first reaction liquid, and control the temperatur...

Embodiment 3

[0052] The synthetic technique of 3-aminopyridine comprises the following synthetic steps:

[0053]Step 1: Preparation of nicotinamide: The equipment for nicotinamide preparation uses a reflux device. Add 60ml of water into a three-necked beaker, and then add 12.5g of 3-aminopyridine and 1g of anhydrous sodium carbonate in sequence, stir while reacting, and slowly heat up to 77°C, and then keep warm for about 6 hours until the end of the reaction. After reaching the end of the reaction, cool to room temperature, stop stirring, and obtain a reaction solution containing nicotinamide for later use.

[0054] The judgment of the reaction end point during the preparation of nicotinamide is the same as in Example 1;

[0055] Step 2: Add the nicotinamide-containing reaction liquid in step 1 into the sodium hydroxide solution, and keep the temperature at 2°C during the addition process; then add the sodium hypochlorite solution and stir to obtain the first reaction liquid, and control ...

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Abstract

The present invention discloses a 3-aminopyridine synthesis process, and relates to the field of aminopyridine compound synthesis, and the 3-aminopyridine synthesis process comprises the following synthesis steps: 1, nicotinamide preparation: 3-cyanopyridine and anhydrous sodium carbonate are added into water, the temperature is raised, a heat preservation reaction is performed, and after the reaction is completed, cooling is performed to room temperature to obtain a nicotinamide-containing reaction liquid; step 2, adding the reaction solution containing nicotinamide into a sodium hydroxide solution, and keeping the lowest temperature at 2 DEG C in the adding process; adding a sodium hypochlorite solution, stirring to obtain a first reaction solution, and controlling the temperature to be 5-8 DEG C in the stirring process; 3, heating the first reaction liquid to 75-80 DEG C, continuing the reaction until the reaction is finished to obtain a second product, and cooling the second product to room temperature for later use; and 4, extracting the second reaction liquid, and carrying out reduced pressure distillation on the extracted liquid to obtain 3-aminopyridine. The method has low requirements on reaction conditions, does not use a metal catalyst compared with the traditional method, is low in cost and is more suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of synthesis of aminopyridine compounds, in particular to a synthesis process of 3-aminopyridine. Background technique [0002] 3-aminopyridine is also known as 3-pyridylamino. Appearance is white to light yellow crystal, it turns orange-red-orange red when exposed to light and heat. In medicine, it is used as an intermediate in the production of gastric ulcer and duodenal ulcer drugs. In terms of pesticides, it is used as a raw material for the fungicide Butiobate. [0003] There is a method for synthesizing 3-aminopyridine recorded in the related art, which is prepared from a halogenated pyridine compound: 3-bromopyridine reacts with allylamine under the catalysis of palladium, and then converts it into 3-aminopyridine. [0004] However, the above-mentioned related technologies have the following defects: most of these reactions require the use of metal catalysts, the cost is high, and wastewater treatment is tro...

Claims

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Application Information

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IPC IPC(8): C07D213/73C07D213/82
CPCC07D213/73C07D213/82
Inventor 张辉
Owner 陕西菲尔特化工有限公司
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