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Method for preparing high-purity borneol from lauraceae extract or blumea balsamifera extract

A technology of extract and aina incense, applied in the fields of chemistry and medicine, can solve the problems of high price and short supply

Inactive Publication Date: 2014-04-30
闻永举
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to utilize cheap Lauraceae extracts, such as natural camphor and its reduction product, borneol camphor extract, large-scale preparation of high-purity D-borneol, to solve the problem of natural borneol (mainly containing D-borneol). ) is gradually becoming popular in the international market, the price is expensive, and the supply exceeds the demand; use the extract of Ainaxiang to prepare high-purity L-borneol, and further improve the quality of L-borneol

Method used

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  • Method for preparing high-purity borneol from lauraceae extract or blumea balsamifera extract
  • Method for preparing high-purity borneol from lauraceae extract or blumea balsamifera extract
  • Method for preparing high-purity borneol from lauraceae extract or blumea balsamifera extract

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Experimental program
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Effect test

Embodiment 1

[0082] Embodiment 1: Prepare high-purity d-borneol by natural camphor or its reduction product (1)-distillation-sublimation method

[0083] Take 17g of aluminum powder (AR), add 5g of anhydrous AlCl 3 (AR), quickly mix, then add 2.0gHgCl 2 (AR), mix well, add isopropanol (AR) 1000ml, under airtight, after about 20min, react rapidly, use condenser to condense if necessary. After 6 hours, react in a water bath for 4 hours, add 120 g of natural camphor, and distill off isopropanol in an air bath at 110°C. Add steam, distill, and dry at room temperature to obtain 100 g of natural camphor reduction products (D-borneol, D-isoborneol, a small amount of natural camphor mixture). Take 4g aluminum powder, add 3.5g anhydrous AlCl 3 Mix quickly, add 200ml of isopropanol, under airtight, reflux in a water bath for 12h, add 100g of the above-mentioned natural camphor reduction product, heat until the natural camphor reduction product dissolves, shake well to form a homogeneous solution. ...

Embodiment 2

[0084] Embodiment 2: Prepare high-purity D-borneol-column chromatography by natural camphor or its reduction products

[0085] Take 17g of aluminum powder, add 5g of anhydrous AlCl 3 , mix quickly, then add 2.0gHgCl 2 , mix well, add 1000ml of isopropanol, under airtight, after about 20min, react quickly, if necessary, use a condenser to condense. After 6 hours, react in a water bath for 4 hours, add 120 g of natural camphor, and distill off isopropanol in an air bath at 110°C. Steam distillation was introduced, condensed water was cooled, and the cooled product was subjected to airtight distillation to remove water to obtain 115 g of natural camphor reduction products (D-borneol, D-isoborneol, a small amount of natural camphor mixture). Take 4g aluminum powder, add 3.5g anhydrous AlCl 3 Mix quickly, add 200ml of isopropanol, under airtight, reflux reaction in a water bath for 12h, add 115g of the above-mentioned camphor reduction product, heat until the camphor reduction p...

Embodiment 3

[0086] Embodiment 3: Prepare high-purity d-borneol-extraction method by natural camphor or its reduced product

[0087] Take 17g of aluminum powder, add 5g of anhydrous AlCl 3 , mix quickly, then add 2.0gHgCl 2 , mix well, add 1000ml of isopropanol, under airtight, after about 20min, react quickly, if necessary, use a condenser to condense. After 6 hours, react in a water bath for 4 hours, add 120 g of natural camphor, and distill off isopropanol in an air bath at 110°C. Distilled with water steam, cooled with condensed water, and the cooled product was distilled to remove water in a closed manner to obtain 114g of natural camphor reduction products (D-borneol, D-isoborneol, a small amount of natural camphor mixture). Take 4g aluminum powder, add 3.5g anhydrous AlCl 3， Mix quickly, add 300ml of isopropanol, under airtight, reflux in a water bath for 12h, add 114g of the above-mentioned natural camphor reduction product, and heat until the natural camphor reduction product d...

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Abstract

The invention discloses a method for preparing high-purity borneol from a lauraceae extract or a blumea balsamifera extract. The method comprises the following steps: the extracts and secondary alcohol-secondary alcohol aluminum with low boiling point or tertiary alcohol-tertiary alcohol aluminum are heated in a closed environment to evaporate low boiling point secondary alcohol or tertiary alcohol, camphor in the extracts is reduced into borneol or isoborneol, continuous heating is performed in the closed environment to generate borneol aluminum and isoborneol aluminum, continuous heating is performed in the closed environment to dehydrate the isoborneol aluminum, and rearrangement is performed to generate camphene, distilling is performed by using vapor to evaporate camphene and borneol, and camphene and borneol are separated by using one or more of an extraction method adopting saturated hydrocarbon such as petroleum ether and polar solvents such as DMSO, a column chromatography method using saturated hydrocarbon such as petroleum ether and silica gel, and a distillation-sublimation method, and the like. By using the method, the high-purity dextroborneol can be prepared from the auraceae extract, and high-purity levogyration borneol can be prepared from the blumea balsamifera extract. The whole process is continuous, smooth, simple to operate, low in cost, environment-friendly, and high in both purity and yield of the borneol, and facilitates industrial production. The lauraceae extract comprises natural camphor, reduzate, plant borneol camphor, cinnamomum longepaniculatum and cinnamomum burmanni extract.

Description

technical field [0001] The invention discloses a method for preparing high-purity borneol from lauraceae extract or Ainaxiang extract, and its field is chemistry and medicine. Background technique [0002] Functions and material basis of borneol, natural borneol, and moxa: All three have the effects of resuscitating the mind, clearing away heat and relieving pain. Heartache, red eyes, mouth sores, sore throat, ear canal discharge and other diseases. The 2010 edition of the Pharmacopoeia stipulates that the quality standard of borneol should not be less than 55.0%, camphor should not exceed 0.50%, heavy metals should not exceed 5ppm, arsenic should not exceed 2ppm, and non-volatile matter should not exceed 10g. 3.5 mg. In percentage calculation, heavy metals, arsenic salts, and non-volatile matter are ignored, and the isoborneol content is 100%-0.50%-55.0%=44.50%, and the isoborneol content in borneol should not exceed 44.50%. The Pharmacopoeia stipulates the quality stand...

Claims

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Application Information

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IPC IPC(8): C07C35/30C07C29/143C07C29/92C07C13/40C07C1/24
CPCC07C29/04C07B2200/07C07C1/327C07C29/143C07C29/92C07C2602/42C07C35/30C07C13/40C07C1/24C07C29/705C07C35/46
Inventor 闻永举申秀丽
Owner 闻永举
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