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Chemical synthesis method of 3-chloro-1-propanol

A technology for chemical synthesis and propanol, applied in chemical instruments and methods, organic chemistry, chemical recycling, etc., can solve the problems of many gas raw materials, high equipment requirements, low reaction yield, etc., achieve low industrialization difficulty, improve efficiency, The effect of easy participation in the reaction

Active Publication Date: 2020-01-10
邹平铭兴化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many existing synthetic routes of 3-chloro-1-propanol, and the following are more mature and have certain industrial value: 1, synthesized by propylene, hydrogen chloride and hypochlorous acid, and the reaction uses many gaseous raw materials, The pressure in the kettle changes greatly, the requirements for equipment are high, the reaction is uncontrollable, and it is dangerous
2. Other synthetic routes such as the synthesis of 1,3-dichloropropene or 1-bromo-3-chloropropane as raw materials are multi-step reactions, the reaction yield is often very low, and the reaction requires the use of hydrogen and high vacuum conditions. dangerous

Method used

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  • Chemical synthesis method of 3-chloro-1-propanol
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  • Chemical synthesis method of 3-chloro-1-propanol

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Embodiment 1

[0031] Such as figure 1 Shown, the chemical synthesis method of described 3-chloro-1-propanol specifically comprises the following steps:

[0032] (1) First put 440kg of 1,3-propanediol, 600kg of hydrochloric acid, and 3kg of benzenesulfonic acid into a 2000L glass-lined kettle with stirring and reflux condensation device, stir and heat up to 90°C, and keep warm for reaction;

[0033] (2) After 3 hours of heat preservation, lower the temperature of the kettle to 50°C, then put 460kg of hydrochloric acid into the kettle, continue to heat up to 90°C and keep it warm for 10 hours, then lower the temperature of the kettle and take samples for GC analysis. When 3-chloro-1-propanol When the content of toluene reached 80%, the feed liquid was squeezed into the still, and 150kg of toluene was thrown into the still to carry out the reaction of heating and reflux with water;

[0034] (3) After the reaction with water is completed, the temperature of the kettle is lowered to room temper...

Embodiment 2

[0038] Such as figure 1 Shown, the chemical synthesis method of described 3-chloro-1-propanol specifically comprises the following steps:

[0039] (1) First put 440kg of 1,3-propanediol, 600kg of hydrochloric acid, and 3kg of benzenesulfonic acid into a 2000L glass-lined kettle with stirring and reflux condensation device, stir and heat up to 90°C, and keep warm for reaction;

[0040] (2) After 3 hours of heat preservation, lower the temperature of the kettle to 50°C, then put 460kg of hydrochloric acid into the kettle, continue to heat up to 90°C and keep it warm for 10 hours, then lower the temperature of the kettle and take samples for GC analysis. When 3-chloro-1-propanol When the content of toluene reached 75%, the feed liquid was squeezed into the still, and 150kg of toluene was thrown into the still to carry out the reaction of heating and reflux with water;

[0041] (3) After the reaction with water is completed, the temperature of the kettle is lowered to room temper...

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Abstract

The invention belongs to the technical field of chemical synthesis, and concretely relates to a chemical synthesis method of 3-chloro-1-propanol. 1,3-propylene glycol reacts with hydrochloric acid with benzenesulfonic acid as a catalyst to synthesize 3-chloro-1-propanol. The method comprises the following steps: 1,3-propylene glycol, a part of hydrochloric acid and benzenesulfonic acid are added into a reaction kettle and are reacted, the remaining hydrochloric acid is added into the reaction kettle, the obtained mixture is continuously reacted until the sampling analysis result shows that thesample is qualified, toluene is added, a heating reflux water-carrying reaction is carried out, the kettle is cooled to room temperature after the water-carrying reaction is completed, an oil phase in the kettle is neutralized to be neutral, the oil phase is pumped into a rectifying kettle, and is rectified until the sampling analysis result shows that the sample is qualified, and the finished product is separated out. The method which adopts the benzenesulfonic acid as the catalyst has the advantages of increase of the reaction efficiency, prevention of excessive chlorination, no generationof high-toxicity and high-pollution three wastes in the reaction, recyclability of byproducts, realization of the comprehensive yield of 95% or above, high conversion rate, high operability, low riskand low industrialization difficulty.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a chemical synthesis method of 3-chloro-1-propanol. Background technique [0002] 3-Chloro-1-propanol is an important intermediate in drug synthesis, which can be used in the synthesis of various drugs, such as: the synthesis of 3-chloropropyl chloroformate, the intermediate of nelfinavir, and the intermediate of the antithrombotic drug clopidogrel body. [0003] At present, there are many existing synthetic routes of 3-chloro-1-propanol, and the following are more mature and have certain industrial value: 1, synthesized by propylene, hydrogen chloride and hypochlorous acid, and the reaction uses many gaseous raw materials, The pressure in the kettle changes greatly, the requirements for equipment are high, the reaction is uncontrollable, and it is dangerous. 2. Other synthetic routes such as the synthesis of 1,3-dichloropropene or 1-bromo-3-chloropropane...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/62C07C29/80C07C31/36
CPCC07C29/62C07C29/80C07C31/36Y02P20/584
Inventor 陈强张鹏张俊玲曹新明孙凡通王涛杜晓阳
Owner 邹平铭兴化工有限公司
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