The chemical synthesis method of 3-chloro-1-propanol
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A technology for chemical synthesis and propanol, applied in chemical instruments and methods, organic chemistry, chemical recycling, etc., can solve problems such as large pressure changes, high equipment requirements, and many gas raw materials, achieving low risk, low industrialization difficulty, The effect of improving efficiency
Active Publication Date: 2022-07-08
邹平铭兴化工有限公司
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[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
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Embodiment 1
[0031] like figure 1 Shown, the chemical synthesis method of described 3-chloro-1-propanol, specifically comprises the following steps:
[0032] (1) 440kg 1,3-propanediol, 600kg hydrochloric acid, 3kg of benzenesulfonic acid are dropped into the 2000L glass-lined still with stirring and reflux condensing device, and stirring is warming up to 90 ℃, insulation reaction;
[0033] (2) after being incubated for 3 hours, reduce the temperature of the still to 50 ° C, drop 460kg of hydrochloric acid into the still, continue to be warming up to 90 ° C and be incubated for 10 hours, reduce the temperature of the still for sampling GC analysis, when 3-chloro-1-propanol When the content of toluene reaches 80%, the feed liquid is pushed into the still, and 150kg of toluene is thrown into the still to carry out the heating and refluxing reaction with water;
[0034] (3) lower the temperature of the still to room temperature after the reaction with water, add sodium bicarbonate and neutral...
Embodiment 2
[0038] like figure 1 Shown, the chemical synthesis method of described 3-chloro-1-propanol, specifically comprises the following steps:
[0039] (1) 440kg 1,3-propanediol, 600kg hydrochloric acid, 3kg of benzenesulfonic acid are dropped into the 2000L glass-lined still with stirring and reflux condensing device, and stirring is warming up to 90 ℃, insulation reaction;
[0040] (2) after being incubated for 3 hours, reduce the temperature of the still to 50 ° C, drop 460kg of hydrochloric acid into the still, continue to be warming up to 90 ° C and be incubated for 10 hours, reduce the temperature of the still for sampling GC analysis, when 3-chloro-1-propanol When the content reached 75%, the feed liquid was pushed into the still, and 150kg of toluene was thrown into the still to carry out the heating and refluxing reaction with water;
[0041] (3) lower the temperature of the still to room temperature after the reaction with water, add sodium bicarbonate and neutralize the o...
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Abstract
The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for chemical synthesis of 3-chloro-1-propanol, wherein benzenesulfonic acid is used as a catalyst, and 1,3-propanediol is reacted with hydrochloric acid to synthesize 3-chloro-1-propanol, The method includes the following steps: firstly put 1,3-propanediol, part of hydrochloric acid and benzenesulfonic acid into the reaction kettle for reaction, then put the remaining hydrochloric acid into the reaction kettle, continue to react until the sampling and analysis are qualified, then put into toluene for heating and refluxing with water After the reaction with water, the temperature of the kettle is lowered to room temperature, the oil phase in the kettle is neutralized to neutrality, the oil phase is pumped into the rectification kettle, and the finished product is separated after rectification until the sampling is qualified. By using benzenesulfonic acid as the catalyst, the present invention improves the reaction efficiency and prevents excessive chlorination, no three wastes with high toxicity and high pollution are generated in the reaction, the by-products can still be recovered and reused, and the comprehensive yield can reach more than 95%. The conversion rate is high, the operability is high, the risk is small, and the difficulty of industrialization is low.
Description
technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a chemical synthesis method of 3-chloro-1-propanol. Background technique [0002] 3-Chloro-1-propanol is an important intermediate in drug synthesis and 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 ones that are more mature and have certain industrial value are as follows: 1. Synthesized from propylene, hydrogen chloride and hypochlorous acid, and this reaction uses many gaseous raw materials, The pressure in the kettle changes greatly, the equipment requirements 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 ...
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