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Synthesis method of (2-hydroxyethyl)pyridine

A technology of hydroxyethylpyridine and picoline, which is applied in the field of synthesis of 2-hydroxyethylpyridine, can solve the problems of high production cost, long reaction time, and low single-pass conversion rate, so as to shorten the reaction time and save production cost , The effect of high conversion rate in one pass

Pending Publication Date: 2020-11-27
SHANGHAI ZHONGXI SUNVE PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved in the present invention is to overcome the shortcomings of the existing 2-hydroxyethylpyridine preparation method, such as long reaction time, low single pass conversion rate and high production cost, and provide a synthetic method of 2-hydroxyethylpyridine

Method used

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  • Synthesis method of (2-hydroxyethyl)pyridine
  • Synthesis method of (2-hydroxyethyl)pyridine
  • Synthesis method of (2-hydroxyethyl)pyridine

Examples

Experimental program
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Embodiment 1

[0041]

[0042] Add 2-picoline (30g, 322mmol), paraformaldehyde (2.04g, 64.4mmol, 95%), water (4.08g, 226mmol) and DABCO (0.36g, 3.22mmol) in the depolymerization flask at 120°C The depolymerization was carried out for 20 minutes, and it was used as the reaction solution to wait for the feed. Connect the stainless steel micro-reaction pipeline with the advection pump, and connect it with a pressure-adjustable backpressure valve, control the pipeline reaction pressure to 4MPa, and connect a 5m-long pre-cooling pipeline at the front end of the backpressure valve. Use reaction solvent water at a flow rate of 1 ml / min to fully rinse the 30-m-long reaction pipeline for 30 minutes, and then blow the reaction pipeline with nitrogen for 30 minutes to fully dry the pipeline. Control the temperature of the heater to 200° C., adjust the flow rate of the pump to 2 ml / min, and pump the reaction liquid to start the reaction. After 8min, the pale yellow liquid product begins to flow out,...

Embodiment 2

[0046] Add 2-picoline (30g, 322mmol), paraformaldehyde (2.04g, 64.4mmol, 95%), water (4.08g, 226mmol) and DABCO (0.36g, 3.22mmol) in the depolymerization flask at 120°C The depolymerization was carried out for 20 minutes, and it was used as the reaction solution to wait for the feed. Connect the stainless steel micro-reaction pipeline with the advection pump, and connect it with a pressure-adjustable backpressure valve, control the pipeline reaction pressure to 4MPa, and connect a 5m-long pre-cooling pipeline at the front end of the backpressure valve. Use reaction solvent water at a flow rate of 1 ml / min to fully rinse the 30-m-long reaction pipeline for 30 minutes, and then blow the reaction pipeline with nitrogen for 30 minutes to fully dry the pipeline. Control the temperature of the heater to 200°C, adjust the flow rate of the pump to 1ml / min, and pump the reaction solution to start the reaction. After 15min, the light yellow liquid product began to flow out, and the liq...

Embodiment 3

[0048] Add 2-picoline (30g, 322mmol), paraformaldehyde (2.04g, 64.4mmol, 95%), water (6.12g, 340mmol) and DABCO (0.36g, 3.22mmol) in the depolymerization flask at 120°C The depolymerization was carried out for 20 minutes, and it was used as the reaction solution to wait for the feed. Connect the stainless steel micro-reaction pipeline with the advection pump, and connect it with a pressure-adjustable backpressure valve, control the pipeline reaction pressure to 4MPa, and connect a 5m-long pre-cooling pipeline at the front end of the backpressure valve. Use reaction solvent water at a flow rate of 2 ml / min to fully rinse the 30-m-long reaction pipeline for 30 minutes, and then blow the reaction pipeline with nitrogen for 30 minutes to fully dry the pipeline. Control the temperature of the heater to 200° C., adjust the flow rate of the pump to 2 ml / min, and pump the reaction liquid to start the reaction. After 8min, the pale yellow liquid product begins to flow out, and the liq...

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Abstract

The invention discloses a synthesis method of (2-hydroxyethyl)pyridine. The preparation method comprises the following step: reacting 2-methylpyridine with formaldehyde in a solvent under a pressure of 2-8 MPa and under the action of organic alkali so as to obtain (2-hydroxyethyl)pyridine, wherein the organic alkali is one or more selected from triethylene diamine, hexamethylenediamine, tetramethyl guanidine, 1,8-diazabicycloundec-7-ene and 1,5,7-triazabicyclo[4.4.0]deca-5-ene. When the method is used for preparing (2-hydroxyethyl)pyridine, reaction time is obviously shortened, a one-way conversion rate is high, and production cost can be saved.

Description

technical field [0001] The invention relates to a synthesis method of 2-hydroxyethylpyridine. Background technique [0002] 2-Hydroxyethylpyridine is a widely used fine chemical product. It can synthesize 2-vinylpyridine and many other fine organic chemical intermediates. It is also widely used in pesticides and medicines, and has high development value. . At present, the synthesis of 2-hydroxyethylpyridine is mainly through the synthesis of paraformaldehyde or formaldehyde aqueous solution and 2-picoline as raw materials. [0003] In the patent application with the publication number CN86103091A, 2-picoline and formaldehyde aqueous solution are used as raw materials, and under the catalysis of benzoic acid or acetic acid, the reaction is carried out at 105°C-128°C for 45-70h, and the single-pass conversion rate reaches 40-60. %, then reclaim the 2-picoline that has not completely reacted, then add new formaldehyde aqueous solution and 2-picoline to make it become the init...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/30
CPCC07D213/30
Inventor 颜国明尹超俞伟叶金星
Owner SHANGHAI ZHONGXI SUNVE PHARMA
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