Separation method suitable for chemical synthesis of salidroside for industrial production

A technology of salidroside and a separation method, applied in the field of salidroside synthesis, can solve the problems of unsuitability for industrial production, cumbersome column separation method, high cost, etc., and achieves reduction of industrial pollution, low production cost, and high production cost. reduced effect

Active Publication Date: 2014-09-17
LIAONING UNIVERSITY
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  • Abstract
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Problems solved by technology

Compared with the traditional method, these two methods have simpler raw materials and shorter steps, but there are still obvious disadvantages. For example, the post...

Method used

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  • Separation method suitable for chemical synthesis of salidroside for industrial production

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Embodiment 1

[0025] 1) In a 250ml eggplant-shaped bottle, add a stirring rod, 4g (1.2eq) of β-D-pentaacetylglucose, 1.18g (1eq) of p-hydroxyphenylethyl alcohol and 4g of 4A molecular sieve, and add dry CH 2 Cl 2 60ml was dissolved, and the reactor was placed on a magnetic stirrer, and slowly added dropwise with 10ml of dichloromethane solution containing 2.67g (1.2eq) of anhydrous tin tetrachloride while stirring at 0°C. After the dropwise addition, stirred at 40°C for 2 hour, stop the reaction, now there is a small amount of p-hydroxyphenylethanol remaining, the color of the solution is slightly light yellow, filter out the molecular sieve, and get the reaction solution containing tetraacetylsalidroside, the liquid phase detection tetraacetylsalidroside conversion rate is 94 %.

[0026] 2) In the reaction liquid, add 50ml of 5% sodium bicarbonate aqueous solution while stirring, after stirring, add diatomaceous earth, filter to remove insoluble matter, take the organic phase (that is, th...

Embodiment 2

[0031] 1) In a 250ml eggplant-shaped bottle, add a stirring rod, 4g (1.2eq) of β-D-pentaacetylglucose, 1.18g (1eq) of p-hydroxyphenylethyl alcohol and 4g of 4A molecular sieve, and add dry CH 2 Cl 260ml was dissolved, and the reactor was placed on a magnetic stirrer. Slowly add a 10ml ether solution containing 0.70g (1.2eq) of boron trifluoride dropwise while stirring at 0°C. After the dropwise addition, stir at room temperature for 2 hours to stop the reaction. At this time, there was a small amount of p-hydroxyphenylethanol remaining, and the color of the solution was slightly light yellow, and the molecular sieve was filtered to obtain a reaction solution containing tetraacetylsalidroside. The conversion rate of tetraacetylsalidroside was 92% according to liquid phase detection.

[0032] 2) In the reaction liquid, add 50ml of 5% sodium bicarbonate aqueous solution while stirring, after stirring, add diatomaceous earth, filter to remove insoluble matter, take the organic pha...

Embodiment 3

[0036] 1) In a 250ml eggplant-shaped bottle, add a stirring bar, 4g (1.2eq) of β-D-pentaacetylglucose, 1.66g (1.2eq) of anhydrous ferric chloride, 1.18g (1eq) of p-hydroxyphenylethyl alcohol and 4A Molecular sieve 4g, add dry CH 2 Cl 2 80ml was dissolved, and the reactor was placed on a magnetic stirrer, and stirred at 15°C for 4 hours to stop the reaction. At this time, there was a small amount of p-hydroxyphenethyl alcohol remaining, and the color of the solution was slightly light yellow. Filtered out molecular sieves to obtain tetraacetyl salidroside In the reaction solution, the conversion rate of tetraacetylsalidroside was 92% by liquid phase detection.

[0037] 2) In the reaction liquid, add 50ml of 5% sodium bicarbonate aqueous solution while stirring, after stirring, add diatomaceous earth, filter to remove insoluble matter, take the organic phase (that is, the dichloromethane phase) in the filtrate, use the organic phase Extract with ionic water until the p-hydroxy...

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Abstract

The invention discloses a separation method suitable for chemical synthesis of salidroside for industrial production. The method comprises the following steps: carrying out a reaction on Beta-D-pent-acetyl glucose and hydroxyphenethyl alcohol under the catalytic action of a lewis acid; and carrying out deacetylation on a generated tetraacetyl salidroside product so as to prepare the salidroside. Thus, the salidroside product is synthesized in a separating manner via an extraction and recrystallization method while a simple and convenient synthesis method is adopted at the same time. Compared with the traditional chemical synthesis process, the method disclosed by the invention is low in cost, high in yield, short in reaction time, simple and simple, convenient and environmentally friendly in synthesis process, thereby being suitable for industrial production, and the raw materials are easily available.

Description

technical field [0001] The invention belongs to the field of pharmaceutical chemical synthesis, and in particular relates to a method for synthesizing and separating salidroside suitable for industrial production. Background technique [0002] Rhodiola is a perennial herbaceous plant of the Sedum family. It mainly grows in areas with an altitude of 1600-4000 meters in high cold, dry and hypoxic, strong ultraviolet radiation, and large temperature difference between day and night. It has strong environmental adaptability and vitality. Rhodiola has been used in China very early, and it is recorded in "Four Medical Codes" and "Compendium of Materia Medica". Salidroside is the main medicinal component of Rhodiola. Various pharmacological effects such as immune regulation and free radical scavenging. [0003] Rhodiola is a plant in the alpine region. Due to the fragile ecology of the plateau and poor regeneration ability, the natural regeneration is very slow. Generally, it take...

Claims

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Application Information

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IPC IPC(8): C07H1/00C07H15/18
Inventor 王洋陈烨姜帆倪晋李萌王琦宋洋宁宝入
Owner LIAONING UNIVERSITY
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