Beta-caryophyllene alcohol derivative as well as preparation method and preparation device thereof

A caryophyllene alcohol and preparation device technology, which is applied in the preparation of organic compounds, carboxylate esters, organic chemical methods, etc., can solve the problems of poor operability and complicated preparation process, and improve the preparation efficiency and reliability. controllability and avoid severe carbonization

Inactive Publication Date: 2019-12-27
CHONGQING MEDICAL & PHARMA COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For this reason, the embodiment of the present invention provides a β-caryophyllene alcohol derivative and its preparation method and preparation device, so as to simplify the entire preparation process from β-caryophyllene to β-caryophyllene alcohol derivative through one-time preparation. 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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  • Beta-caryophyllene alcohol derivative as well as preparation method and preparation device thereof
  • Beta-caryophyllene alcohol derivative as well as preparation method and preparation device thereof
  • Beta-caryophyllene alcohol derivative as well as preparation method and preparation device thereof

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preparation example Construction

[0066] Such as figure 1 As shown, the invention provides a kind of preparation method of β-caryophyllenol derivative, comprising:

[0067] 100. In the condition of an ice-water bath and the presence of the first solvent, add concentrated sulfuric acid to β-caryophyllene and mix to obtain a mixed solution;

[0068] 200. After stirring and mixing the above mixed solution 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, and the first organic layer is obtained by separation;

[0069] 300. Distill the first organic layer, collect the distillate, and dry to obtain a crude product;

[0070] 400. In the presence of the second solvent, 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 obtain second...

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. (obtaining product A1 is 5.93g, productive rate 74.79%)

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Abstract

The embodiment of the invention discloses a beta-caryophyllene alcohol derivative as well as a preparation method and a preparation device thereof. The preparation device comprises a cold and hot water storage tank (1) with a containing cavity (101), a mixing unit (2) at least partially arranged in the containing cavity (101), an elution column and a stirring backflow unit (3), wherein the elutioncolumn and the stirring backflow unit (3) are arranged outside the cold and hot water storage tank (1). The whole preparation process from beta-caryophyllene to the beta-caryophyllenol derivative isachieved in one vessel, the whole preparation process is simplified, the overall controllability of the preparation device is adjusted on the basis of simplification, and therefore 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-caryophyllenol derivatives, in particular to a β-caryophyllenol derivative and its preparation method and preparation device. 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 method of extracting n...

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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