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Preparation method of 2-ethoxyl pyridina

A technology of hydroxyethyl pyridine and picoline, which is applied in the field of preparation of 2-hydroxyethyl pyridine, can solve the problems of high production cost, low production efficiency, low yield and the like, and achieves low production cost, high production efficiency, The effect of high product yield

Inactive Publication Date: 2012-10-17
SHANDONG TIANYI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of this invention is to provide a new method for the synthesis of 2-hydroxyethylpyridine, to overcome the defects of low production efficiency, low yield and high production cost in the prior art

Method used

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  • Preparation method of 2-ethoxyl pyridina

Examples

Experimental program
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Embodiment 1

[0020] (1) In a 1000ml four-neck flask equipped with a thermometer, a magnetic stirrer, and a reflux condenser, add 93.13g of 2-picoline, 107.12g of lithium diisopropylamide, and 176.2ml of tetrahydrofuran, and fill the reaction system with Nitrogen protection was carried out, and the reaction was carried out under the condition of stirring and temperature of -60° C. for 1 hour to obtain a reaction liquid. (2) Add 27.60g of paraformaldehyde to the above reaction solution, stir and react for 1 hour under the reaction conditions of 10°C temperature, then add 18g of water dropwise under the above reaction conditions, and the drop time is 0.5 hours. The reaction was continued for 0.5 hour under the temperature condition of 10° C. to obtain the product liquid. (3) Add calcium sulfate to the above-mentioned product liquid, carry out dehydration treatment, filter the product liquid after removing moisture, carry out vacuum distillation on the filtrate under the conditions of temperat...

Embodiment 2

[0022] (1) In a 1000ml four-neck flask equipped with a thermometer, a magnetic stirrer, and a reflux condenser, add 93.13g of 2-picoline, 160.68g of lithium diisopropylamide, and 220.3ml of tetrahydrofuran, and fill the reaction system with Protected by nitrogen, the mixture was stirred and reacted for 2.5 hours at -30°C to obtain a reaction liquid. (2) Add 36.32g of paraformaldehyde to the above reaction solution, stir and react for 3 hours under the reaction conditions of 30°C, then add 21.6g of water dropwise under the above reaction conditions for 1 hour, after the addition is completed The reaction was continued at 40°C for 1 hour to obtain a product solution. (3) Add aluminum oxide to the above product liquid, perform water removal treatment, filter the product liquid after removing water, and carry out vacuum distillation on the filtrate at a temperature of 65°C and -0.859~-0.98MPa to remove tetrahydrofuran, That is, the target product 2-hydroxyethylpyridine was obtain...

Embodiment 3

[0024] (1) In a 1000ml four-neck flask equipped with a thermometer, a magnetic stirrer, and a reflux condenser, add 93.13g of 2-picoline, 214.24g of lithium diisopropylamide, and 440.6ml of tetrahydrofuran, and fill the reaction system with Nitrogen protection was carried out, and the reaction was carried out under the condition of stirring and -10° C. for 4 hours to obtain a reaction solution. (2) Add 44.98g of paraformaldehyde to the above reaction solution, stir and react under the reaction conditions of 60°C for 5 hours, and then under the above reaction conditions, add 27g of water dropwise for 1.5 hours. The reaction was continued at 60°C for 1.5 hours to obtain a product solution. (3) Add 4A molecular sieves to the above product liquid, perform water removal treatment, filter the product liquid after removing water, and conduct vacuum distillation on the filtrate at a temperature of 60°C and -0.859~-0.98MPa to remove tetrahydrofuran, That is, the target product 2-hydro...

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Abstract

The invention discloses a preparation method of 2-ethoxyl pyridina, which comprises the steps of: (1) using tetrahydrofuran as a solvent, enabling 2-methyl pyridine and organic alkali to completely react in the solvent at -60-60 DEG C to prepare a reaction liquid; (2) adding paraformaldehyde into the reaction liquid, agitating and reacting for 0.5-5 hours at 10-60 DEG C, then dropping water into the mixture under the reaction condition, and agitating continuously and reacting for 0.5-1 hours at 10-60 DEG C after dropping water to prepare a product liquid; and (3) removing water in the product liquid, then removing tetrahydrofuran in the product liquid to obtain the 2-ethoxyl pyridine. The method provided by the invention is simple in process operation, short in synthesizing time of product, low in production cost, high in production efficiency, less in secondary reaction, high in product yield and high in purity.

Description

technical field [0001] The invention relates to a preparation method of pyridine compounds, in particular to a preparation method of 2-hydroxyethylpyridine. Background technique [0002] 2-Hydroxyethylpyridine is a high-tech, high-value-added fine chemical product that has been widely used, through which vinylpyridine and many other fine organic chemical intermediates can be synthesized. 2-Hydroxyethylpyridine is a colorless or light yellow transparent liquid with a molecular weight of 123.15. It is miscible with ethanol and ether, soluble in water, and easy to absorb moisture. It has a wide range of uses in polymer materials, surfactants, medicines, pesticides, etc., and has high development value. [0003] [0004] Above-mentioned equation is the synthetic equation of 2-hydroxyethylpyridine, and this reaction is a kind of reversible equilibrium reaction, and single pass conversion rate is very low. Initially, the synthesis of 2-hydroxyethylpyridine was carried out by ...

Claims

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Application Information

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IPC IPC(8): C07D213/30
Inventor 闫晓红李善清赵庭栋杨海燕徐文辉孟烨李远超
Owner SHANDONG TIANYI CHEM
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