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Method for synthesizing cyclopentanol by continuous flow microreactor

A micro-reactor, micro-channel reactor technology, applied in chemical instruments and methods, sulfate preparation, chemical/physical/physical-chemical processes, etc., can solve problems such as low conversion rate of raw materials, many by-products, and environmental pollution. , to achieve the effect of improving the conversion rate of raw materials, low total cost, low energy consumption and labor cost

Pending Publication Date: 2022-04-01
湖南华腾医药有限公司
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Problems solved by technology

[0007] Aiming at the above-mentioned preparation method of cyclopentanol kettle reaction, there are technical problems such as low conversion rate of raw materials, high risk, many by-products and environmental pollution, etc., the present invention provides a continuous flow micro-reaction synthesis of cyclopentanol The method, by using the continuous flow process, compared with the batch process using the traditional tank reactor, this method has the characteristics of high yield, less post-treatment wastewater, low energy consumption and labor costs, low total project cost, and increased production capacity

Method used

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  • Method for synthesizing cyclopentanol by continuous flow microreactor
  • Method for synthesizing cyclopentanol by continuous flow microreactor
  • Method for synthesizing cyclopentanol by continuous flow microreactor

Examples

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Effect test

Embodiment 1

[0052] The preparation of embodiment 1 compound B

[0053]

[0054] Put 1 mol of cyclopentene in storage bottle A, 1.2 mol of 80% sulfuric acid aqueous solution in storage bottle B, set the reaction temperature to 30°C, and use two plunger-type metering pumps for the materials in A and B bottles respectively Pump into the microchannel responder at a flow rate of 1:1.2, the residence time is 2 minutes, collect the liquid product, and monitor the complete reaction by HPLC. After the reaction liquid flows out, it enters the post-processing system. After extraction, drying, and removal of the organic solvent, compound B is obtained. , with a purity of 99.5% and a yield of 94%.

Embodiment 2

[0057] The preparation of embodiment 2 cyclopentanols

[0058]

[0059] Put the compound B and water obtained in Example 1 in the liquid storage bottle C, set the reaction temperature to 90°C, and pump the materials in the compound B and C bottles into the microchannel at a flow rate of 1:1 with two plunger-type metering pumps In the reactor, the residence time is 10min, the liquid product is collected, and the reaction is completely monitored by HPLC. After the reaction liquid flows out, it enters the post-processing system. After extraction, drying, and removal of the organic solvent, cyclopentanol is obtained with a purity of 98.5%. 96%.

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Abstract

The invention relates to a continuous flow micro-reaction synthesis method of cyclopentanol, and belongs to the technical field of medicine preparation. According to the preparation method, cyclopentanol is technically optimized by adopting a continuous flow microreactor technology, cyclopentene is taken as a starting material, and cyclopentanol is synthesized through reactions such as sulfonation reaction and hydrolysis reaction. Meanwhile, the influence of factors such as the material molar ratio, the reaction retention time and the reaction temperature involved in the technological process on the yield and the purity is investigated, and the optimal technological condition is determined. The optimization process has the characteristics of high yield, less post-treatment wastewater, low energy consumption, low labor cost, low total project cost and capacity improvement.

Description

technical field [0001] The invention relates to the technical field of medicine preparation, in particular to a method for synthesizing cyclopentanol in a continuous flow microreactor. Background technique [0002] Cyclopentanol (Cyclopentanol), CAS No.: 96-41-3, is mainly used as a solvent and dye intermediate for fragrances and pharmaceuticals. Its chemical structural formula is shown in following formula I: [0003] [0004] The method of cyclopentanol reported in the prior art obtains cyclopentanol by cyclopentene after two-step reaction of addition and hydrolysis, wherein, the first step causes great harm to safety because cyclopentene is inflammable and explosive. pressure. In the second step of hydrolysis reaction, there are many side reactions, low yield, and a lot of waste water, which puts a lot of pressure on environmental protection. [0005] The continuous flow reactor is a chemical reaction that occurs in a tiny space. The average size of the channel is 1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/12C07C35/06C07C303/24C07C305/20B01J19/00
Inventor 王芳芳许慧陈芳军
Owner 湖南华腾医药有限公司
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