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Preparation method of special chromatographic medium for separating cannabidiol

A technology of cannabidiol and cannabidiol, which is applied in the field of chromatographic media, can solve the problems of low yield, cumbersome steps, and inability to produce in large quantities, and achieve the effects of high purity, simple process, and easy operation

Pending Publication Date: 2022-06-10
SOOCHOW HIGH TECH CHROMATOGRAPHY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] There are many deficiencies in the existing process for producing cannabidiol, such as low yield, cumbersome steps, and inability to prepare in large quantities.

Method used

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  • Preparation method of special chromatographic medium for separating cannabidiol
  • Preparation method of special chromatographic medium for separating cannabidiol
  • Preparation method of special chromatographic medium for separating cannabidiol

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Embodiment 1

[0032] The specific steps of the present invention are as follows:

[0033] (1) Take 15g of monoplasmic bromine, 3g of cannabidiol, 0.1g of glacial acetic acid, mixed reaction;

[0034] (2) Weigh 30g of porous amino silicon balls with a particle size of 50 μm, add to xylene, stir well to make it completely wet;

[0035] (3) Brominated hypocandiol intermediates and 0.1g 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide were then added to the above solution, 75 °C reaction.

[0036] After the reaction is completed, it is filtered and dried, that is, the special chromatographic separation medium is obtained and the column is loaded.

[0037] Pillar: 15×310mm, 50 μm,

[0038] Wavelength: 210nm

[0039] Mobile phase: methanol - water

[0040] Flow rate: 10.6ml / min

[0041] Take 10 g of crude hypocandiol extracted by solvent method and analyze it with C18 reversed-phase column, see Figure 3 。 Separation and purification of subnabinol was performed with a loaded preparative column to obtain 1...

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Abstract

The invention relates to a preparation method of a special chromatographic medium for separation of sec-cannabidiol, which comprises the following steps: (1) reacting elemental bromine, sec-cannabidiol and a catalyst to obtain a brominated sec-cannabidiol intermediate; (2) adding a certain amount of porous amino silicon balls into an organic solvent, and fully stirring to completely wet the porous amino silicon balls; and (3) adding the brominated cannabidiol intermediate and a catalyst into the solution, and heating to react. And after the reaction is finished, filtering and drying to obtain the special chromatographic separation medium. According to the invention, secondary cannabidiol is bonded to a silicon ball to form the surface modified silica gel chromatographic filler; the medium has high-selectivity adsorption retention on the cannabidiol, has the advantages of good selectivity and low cost, and is suitable for industrial purification of the cannabidiol.

Description

Technical field [0001] The present invention relates to the field of chromatographic media technology, in particular, is a preparation method of a special chromatographic medium for the separation of hypocandiol. Background [0002] Cannabis is a cannabis family, cannabis plants, commonly known as hemp, line hemp, hemp, cultivation history, has an important agricultural and medicinal value, cannabis contains a toxic ingredient tetrahydrocannabinol (THC) can make people hallucinogenic addiction, often used by people to refine drugs, has been banned for a long time. [0003] Cannabis is now widely recognized as having significant benefits for a variety of medical uses, such as cannabis is often widely used by society to treat a variety of diseases, diseases, and symptoms, including nausea, pain, glaucoma, loss of appetite, mucosal inflammation, neurodegenerative diseases, epilepsy, diabetes, leprosy, etc., as well as the usual fever, cough, obesity, asthma, urinary tract infections...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/30B01J20/32B01J20/22B01D15/26C07C37/82
CPCB01J20/28021B01J20/28004B01J20/28054B01J20/22B01J20/3085B01J20/32B01J20/3214B01D15/265B01D15/165C07C37/82C07C39/23
Inventor 张维冰李笃信戈兆松
Owner SOOCHOW HIGH TECH CHROMATOGRAPHY
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