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Preparation method and preparation device of beta-caryophyllene alcohol derivative

A technology for caryophyllene alcohol and a preparation device is applied in the preparation of organic compounds, the preparation of carboxylic acid esters, organic chemical methods, etc., and can solve the problems of complicated preparation process and poor operability, and achieves improved controllability and improved operability. Preparation efficiency, avoid the effect of conversion

Active Publication Date: 2020-11-06
CHONGQING MEDICAL & PHARMA COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For this reason, the embodiment of the present invention provides a preparation method of β-caryophyllene alcohol derivatives and a preparation device thereof, so as to simplify the entire preparation process from β-caryophyllene to β-caryophyllene alcohol derivatives at one time. The preparation process, and adjust the overall controllability of the preparation device on the basis of simplification, so as to solve the problems of complicated preparation process and poor operability

Method used

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  • Preparation method and preparation device of beta-caryophyllene alcohol derivative
  • Preparation method and preparation device of beta-caryophyllene alcohol derivative
  • Preparation method and preparation device of beta-caryophyllene alcohol derivative

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preparation example Construction

[0061] like figure 1 As shown, the invention provides a kind of preparation method of β-caryophyllenol derivative, comprising:

[0062] 100. Add concentrated sulfuric acid to β-caryophyllene in the presence of solvent A in an ice-water bath and mix to obtain a β-caryophyllene mixed solution;

[0063] 200. After stirring and mixing the β-caryophyllene mixture at a temperature not higher than 5°C for 8-12 hours, continue to add a saturated sodium carbonate solution dropwise to it in an ice-water bath until the layers are separated to obtain the second an organic layer;

[0064] 300. Distill the first organic layer, collect the distillate, and dry to obtain a crude product;

[0065] 400. In the presence of solvent B, mix the crude product, carboxylic acid and catalyst, stir and reflux for 12-24 hours, then continue to add saturated sodium carbonate solution dropwise to it in an ice-water bath until the layers are separated, and the second organic layer;

[0066] 500. The seco...

Embodiment 1

[0109] Fill ice water into the cold and hot water storage tank, add 5g (0.02447mol) β-caryophyllene and 10mL ether to the first storage cylinder, start the stirring paddle to rotate and stir; add 2g of 98% concentrated sulfuric acid to the second storage In the cylinder, slowly push the sealing plate through the air pump until the sulfuric acid enters the connecting pipe; continue to stir for 10h under this condition, then add saturated sodium carbonate dropwise through the titration port to separate layers, open the discharge pipe, collect the first organic layer, distill and dry , get the crude product;

[0110] Mix the above-mentioned crude product, 0.02mol acetic acid and 180mL petroleum ether into the first cylinder for stirring, mix 5mL of 4-dimethylaminopyridine and 20mL petroleum ether into the second cylinder, push it into the connecting pipe for further mixing, Feed through the discharge pipe into the stirring reflux unit and stir and reflux for 18 hours, then import...

Embodiment 2

[0112] The operation was carried out as in Example 1, except that benzoic acid was used instead of acetic acid, and the β-caryophyllenol derivative A2 was collected (5.93 g of product A1, yield 74.79%).

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Abstract

The embodiment of the invention discloses a preparation method and a preparation device of a beta-caryophyllene alcohol derivative. The preparation method comprises the following steps: mixing and stirring beta-caryophyllene and concentrated sulfuric acid, carrying out a reaction until layering, taking an organic layer, drying, mixing the dried crude product, carboxylic acid and a catalyst, carrying out stirring reflux, continuously taking the organic layer, washing, and drying to directly prepare the beta-caryophyllenol derivative. The preparation device comprises a cold and hot water containing groove with a containing cavity, a material mixing unit at least partially arranged in the containing cavity, an elution column and a stirring reflux unit, wherein the elution column and the stirring reflux unit are arranged outside the cold and hot water containing groove. According to the invention, the whole preparation process from beta-caryophyllene to the beta-caryophyllene alcohol derivative is prepared at a time, the whole preparation process is simplified, and the overall controllability of the preparation device is adjusted on the basis of simplification, so that the problems that the preparation process is complex, and operability is not high are solved.

Description

technical field [0001] The embodiment of the present invention relates to the technical field of preparation of β-caryophyllene alcohol derivatives, and specifically relates to a preparation method and a preparation device of β-caryophyllene alcohol derivatives. Background technique [0002] β-Caryophyllenol, also known as syringenol, is a sesquiterpene alcohol compound with strong physiological activity. It is used in many fields such as food seasoning or medicine, but its derivatives are rare various reports. Since its derivatives (for example, ester derivatives) have similar structures, different structures can be obtained through the replacement of substituents, and some other physiologically active substances may be obtained. [0003] However, since β-caryophyllenol generally exists in some plants, it is necessary to extract essential oils from plants and then further process and separate them. Not only is the output scarce, but the cost is high. At the same time, this...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/145C07C69/14C07C69/78C07C201/12C07C205/57
CPCC07B2200/07C07C29/48C07C67/08C07C69/14C07C69/145C07C69/78C07C201/12C07C205/57C07C2602/32C07C35/23
Inventor 徐露黄彦苏湲淇
Owner CHONGQING MEDICAL & PHARMA COLLEGE
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