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Method for preparing diosmin by adopting continuous flow microreactor

A technology of microreactor and diosmin, which is applied in the fields of chemical instruments and methods, chemical/physical/physicochemical reactors, preparation of sugar derivatives, etc., can solve the problem of greater harm to the environment and operators, long reaction time, Eliminate the strong irritating smell of pyridine and other problems, and achieve the effect of enhanced intrinsic safety and safe reaction process

Pending Publication Date: 2021-11-26
XIHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of producing hesperidin through the mechanism of dehydrohalogenation after halogenation (iodine or bromine), the solvent is usually pyridine, which has a strong pungent smell and is more harmful to the environment and operators during the production process. Big
In addition, the reaction time of the traditional process is as long as 8 to 20 hours, which is time-consuming and energy-consuming

Method used

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  • Method for preparing diosmin by adopting continuous flow microreactor
  • Method for preparing diosmin by adopting continuous flow microreactor
  • Method for preparing diosmin by adopting continuous flow microreactor

Examples

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Effect test

Embodiment 1

[0031] Example 1. Preparation of Diosmin by Continuous Flow Microreaction under Pressurization in the Present Invention

[0032] The specific method for preparing diosmin in a continuous flow microreactor under pressure is: adopt Corning microchannel continuous flow reactor (Corning lab-reactor, single module, liquid holding volume 2.7ml, two inlets and one outlet, heat exchange Oil pump rotation number 3500) as reaction equipment, and increase back pressure valve in reactor to increase system pressure, back pressure pressure is 10Bar. Hesperidin was formulated into a hesperidin solution with a concentration of 100mg / ml using an alkaline solvent, and iodine was formulated into an iodine solution with a concentration of 46mg / ml. The molar ratio and a certain flow rate are respectively injected into the reactor, and then the reaction is carried out to obtain a reaction liquid. The pH of the reaction solution was adjusted to neutral with 1 mol / L hydrochloric acid, and after bein...

Embodiment 2

[0039] Example 2, Preparation of Diosmin by Continuous Flow Microreaction under Pressurization in the Present Invention

[0040] The specific method for preparing diosmin in a continuous flow microreactor under pressure is: adopt Corning microchannel continuous flow reactor (Corning lab-reactor, single module, liquid holding volume 2.7ml, two inlets and one outlet, heat exchange Oil pump rotation number 3500) as reaction equipment, and increase back pressure valve in reactor to increase system pressure, back pressure pressure is 10Bar. Hesperidin was formulated into a hesperidin solution with a concentration of 100 mg / ml using an alkaline solvent, and iodine was formulated into an iodine solution with a concentration of 46 mg / ml. The molar ratio was stirred and mixed under normal pressure at 10° C. for 30 minutes, and then injected into the reactor at a certain flow rate for reaction to obtain a reaction liquid. The pH of the reaction solution was adjusted to neutral with 1 m...

Embodiment 3

[0046] Example 3, Preparation of Diosmin by Continuous Flow Microreaction under Normal Pressure of the present invention

[0047] The specific method for preparing diosmin in a continuous flow microreactor under normal pressure is: adopt Corning microchannel continuous flow reactor (Corning lab-reactor, single module, liquid holding volume 2.7ml, two inlets and one outlet, heat exchange Oil pump revolutions 3500) as reaction equipment. Hesperidin is formulated into a hesperidin solution with a concentration of 100mg / ml using an alkaline solvent, and iodine is formulated into an iodine solution with a concentration of 46mg / ml; The molar ratio and a certain flow rate are respectively injected into the reactor, and then the reaction is carried out to obtain a reaction liquid. The pH of the reaction solution was adjusted to neutral with 1 mol / L hydrochloric acid, and after being diluted with DMSO to constant volume, it was analyzed by HPLC to determine the yield of the product di...

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Abstract

The invention provides a method for preparing diosmin by adopting a continuous flow microreactor, and belongs to the technical field of chemical synthesis. The method comprises the following steps: dissolving hesperidin and iodine in an alkaline solvent, and introducing into a continuous flow microreactor for reaction, thereby obtaining the hesperidin; wherein a molar ratio of the hesperidin to the iodine is 1: (1-1.6). According to the method, product conversion rate and yield which are equivalent to production conditions of a traditional process are realized, reaction time is shortened to 2.7 minutes from 8-20 hours of the traditional process, the reaction process is safer, more efficient and quicker, therefore, intrinsic safety of diosmin industrial production is realized, and market competitiveness is further enhanced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing diosmin by using a continuous flow microreactor. Background technique [0002] Diosmin, also known as diosmin, is a pure natural flavonoid glycoside compound, which has been used for more than 30 years as a vascular protective agent and a therapeutic agent for chronic venous diseases. Diosmin is a dehydrogenation product of hesperidin, which has a vitamin P-like effect and can reduce the permeability of capillaries. It causes a stronger constriction effect on veins than other drugs such as rutin. When the body is acidosis, it can still Increases the tone of the veins. Diosmin can also enhance red blood cell flow, reduce microcirculatory stasis, and is used as an adjuvant treatment for the prevention and treatment of hypertension and arteriosclerosis. Therefore, diosmin is an important class of drugs for the treatment of cardiovascul...

Claims

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Application Information

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IPC IPC(8): C07H1/00C07H17/07B01J19/00
CPCC07H1/00C07H17/07B01J19/0093
Inventor 钱珊王周玉宋巧赵卓君陈建军杨胜
Owner XIHUA UNIV
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