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2-amino-3-hydroxypyridine and its preparation method and purification method

A technology of hydroxypyridine and hydroxypyridine sulfonate, which is applied in the direction of organic chemistry, can solve the problems of high raw material prices and low yields, and achieve the effects of high prices, avoiding side reactions, and promoting efficiency

Active Publication Date: 2020-03-24
成家钢
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The embodiment of the present application provides a kind of 2-amino-3-hydroxypyridine and its preparation method and refining method, so as to improve the problems of high raw material price and low yield in the background technology

Method used

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  • 2-amino-3-hydroxypyridine and its preparation method and purification method

Examples

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Effect test

Embodiment 1

[0041]A preparation method of brown 2-amino-3-hydroxypyridine, which comprises:

[0042] Add 350g of water into the first reaction vessel, add 20g of furfural, stir and cool down to 0°C, and start to introduce chlorine gas to carry out the ring-opening reaction. The conditions of the ring-opening reaction include: introducing chlorine gas under continuous stirring, while keeping the reaction temperature at 0-10°C, and the rate of introducing chlorine gas at 2.5-3g / 10min, wherein furfural is added every 20 minutes after the chlorine gas is passed. , add three times altogether, add 10g each time, during, feed chlorine 37g altogether.

[0043] Transfer the mixed liquid agent obtained after the ring-opening reaction to the second reaction container, drop the liquid alkali after cooling to 0°C, adjust the pH of the mixed liquid agent to keep at 1.5-2, and keep the pH of the mixed liquid agent at 1.5-2 The temperature of the mixed solution is 0-10°C, and the time for dropping is ab...

Embodiment 2

[0050] A white 2-amino-3-hydroxypyridine obtained by refining the brown 2-amino-3-hydroxypyridine provided in Example 1 by the following refining method, the refining method comprising:

[0051] Add 45g of brown 2-amino-3-hydroxypyridine obtained in Example 1 into the fourth reaction vessel, add 200ml of dimethylformamide, heat up to 100°C±2°C for 30min, filter while it is hot, and add the filtrate to the fifth In the reaction vessel, the temperature was rapidly cooled to -5°C using an ice-salt bath, and filtered to obtain a white solid.

[0052] Add all the white solid to the sixth reaction vessel, add 200ml of methanol to raise the temperature and reflux for 1 hour, cool down to -5°C, filter, and dry to obtain dry white 2-amino-3-hydroxypyridine.

[0053] Among them, 40g of dry white 2-amino-3-hydroxypyridine has a melting point of 172-174°C. As determined by high performance liquid chromatography, the purity of white 2-amino-3-hydroxypyridine is 99.9%. Calculated, the yiel...

Embodiment 3

[0055] A kind of preparation method of brown 2-amino-3 hydroxypyridine, it comprises:

[0056] Add 370g of water into the first reaction vessel, add 19g of furfural, stir and cool down to 0°C, and start to introduce chlorine gas to carry out the ring-opening reaction. The conditions of the ring-opening reaction include: feeding chlorine gas under continuous stirring, while keeping the reaction temperature at 0-8°C, and the feeding rate of chlorine gas is 2.6-3g / 10min, wherein furfural is added every 20 minutes after chlorine gas feeding , add four times altogether, add 8g each time, during, feed chlorine 39g altogether.

[0057] Transfer the mixed liquid agent obtained after the ring-opening reaction to the second reaction container, drop the liquid alkali after cooling to 0°C, adjust the pH of the mixed liquid agent to keep at 1.5-2, and keep the pH of the mixed liquid agent at 1.5-2 The temperature of the mixed solution is 0-8°C, and the time for dropping is about 2 hours. ...

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Abstract

The invention provides 2-amino-3-pyridone as well as a preparation method and a preparation method thereof, and relates to the field of chemical reagent analysis. The preparation method of the 2-amino-3-pyridone comprises the following steps of introducing chlorine gas or bromine into a furfural water solution to perform loop opening reaction; reacting obtained mixed liquid with an ammonia sulfamate solution to obtain 2-amino-3-pyridone sulfonate; hydrolyzing the 2-amino-3-pyridone sulfonate under the basic condition to obtain brown 2-amino-3-pyridone with the yield being higher than 75 percent. The yield is effectively improved. The furfural is used as raw materials; the cost is effectively reduced. Through refining by a refining method provided by the invention, the white 2-amino-3-pyridone is obtained; the yield of the white 2-amino-3-pyridone is greater than or equal to 70 percent; the purity is higher than 99 percent.

Description

technical field [0001] This application relates to the field of chemical reagent synthesis, in particular, to a 2-amino-3-hydroxypyridine and its preparation method and purification method. Background technique [0002] 2-Amino-3-hydroxypyridine has a wide range of uses, mainly used as pharmaceutical intermediates, such as the preparation of prostate synthase inhibitors, anti-inflammatory drugs, painkillers, antipyretic and pain-relieving tablets, and raw materials for antibacterial drugs; it is also used for the preparation of veterinary drug methyl Pyridinephos; used in the preparation of 2-(BOC-amino)-3-hydroxypyridine; it is also a major ingredient in hair dyes. [0003] At present, there are mainly two kinds of preparation methods for 2-amino-3-hydroxypyridine: 2-nitro-3-hydroxypyridine hydrogenation reduction method, and 3-hydroxypyridine high-pressure ammonia ratio method. The common characteristics of these two methods are The price of the raw material is high, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 成家钢
Owner 成家钢
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