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Preparation method of 4-pyridol

A technology of pyridine phenol and pyridine, applied in the field of preparation of 4-pyridine phenol, can solve problems such as large by-products and long reaction time, and achieve the effects of saving production cost, shortening reaction time and high purity

Inactive Publication Date: 2014-03-26
常熟市联创化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of traditional synthesis of 4-pyridinol, a large number of by-products will be produced, and the reaction time is long

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A kind of preparation method of 4-pyridinol is provided, comprising the steps of:

[0014] (1) Put pyridine and ethyl acetate into a microwave oven for microwave heating. The temperature of the microwave oven is set at 76°C. During the reaction, thionyl chloride is added dropwise to the reactant. The reaction time is 20°C. The reaction is taken out and processed to obtain N-(4-pyridyl)pyridine hydrochloride;

[0015] (2) Mix and heat N-(4-pyridyl)pyridine hydrochloride with water, add potassium hydroxide or sodium hydroxide to adjust the pH value to 8.5, there is precipitation, filter and adjust the pH value to 4.5 with sulfuric acid, and then Treatment affords 4-pyridinol.

Embodiment 2

[0017] A kind of preparation method of 4-pyridinol is provided, comprising the steps of:

[0018] (1) Put pyridine and ethyl acetate into a microwave oven for microwave heating. The temperature of the microwave oven is set at 70°C. During the reaction, thionyl chloride is added dropwise to the reactant. The reaction time is 30°C. The reaction is taken out and processed to obtain N-(4-pyridyl)pyridine hydrochloride;

[0019] (2) Mix and heat N-(4-pyridyl)pyridine hydrochloride with water, add potassium hydroxide or sodium hydroxide to adjust the pH value to 8, there is precipitation, filter and adjust the pH value to 4.8 with sulfuric acid, and then Treatment affords 4-pyridinol.

Embodiment 3

[0021] A kind of preparation method of 4-pyridinol is provided, comprising the steps of:

[0022] (1) Put pyridine and ethyl acetate into a microwave oven for microwave heating. The temperature of the microwave oven is set at 80°C. During the reaction, thionyl chloride is added dropwise to the reactant. The reaction time is 27°C. The reaction is taken out and processed to obtain N-(4-pyridyl)pyridine hydrochloride;

[0023] (2) Mix and heat N-(4-pyridyl)pyridine hydrochloride with water, add potassium hydroxide or sodium hydroxide to adjust the pH value to 7.5, there is precipitation, filter and then adjust the pH value to 5 with hydrochloric acid, and then Treatment affords 4-pyridinol.

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PUM

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Abstract

The invention discloses a preparation method of 4-pyridol. The method comprises the following steps: mixing pyridine and ethyl acetate, treating the mixture with microwave in a microwave oven, dropwise adding thionyl chloride into the reactants during the reaction process, taking out the reactants and conducting posttreatment to obtain N-(4-pyridyl) pyridine hydrochloride; and mixing and heating N-(4-pyridyl) pyridine hydrochloride with water, adding alkaline substances to adjust the pH value to 7.5-8.5, precipitating precipitate, filtering the precipitate, adjusting the pH value to 4.5-5 with acidic substances and conducting posttreatment to obtain 4-pyridol. Through the above way, the preparation method of 4-pyridol provided by the invention employs a microwave method for synthesis, has simple synthetic process, greatly shortens the reaction time and saves the cost of production. The obtained 4-pyridol has high purity, almost contains no by-product, does not need other treatment process, and can be directly applied to the subsequent production.

Description

technical field [0001] The invention relates to the field of fine organic synthesis, in particular to a preparation method of 4-pyridinol. Background technique [0002] The molecular formula of 4-pyridinol is C 5 h 5 NO, with a molecular weight of 95.1, has a certain degree of irritation, and has a great stimulating effect on the eyes, respiratory system and skin. 4-Pyridinol is an important intermediate in organic synthesis, widely used in medicine, pesticides, etc. body. In the process of traditional synthesis of 4-pyridinol, a large number of by-products will be produced, and the reaction time is long. Contents of the invention [0003] The technical problem mainly solved by the present invention is to provide a preparation method of 4-pyridinol, which is simple to operate and safe and reliable. [0004] In order to solve the above-mentioned technical problems, a technical scheme adopted in the present invention is: a kind of preparation method of 4-pyridinol is pr...

Claims

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Application Information

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IPC IPC(8): C07D213/68
CPCC07D213/68
Inventor 陈雪平
Owner 常熟市联创化学有限公司