Preparation method of high-purity levorotatory borneol

A high-purity levoborneol technology, applied in the field of pharmacy, can solve the problems that do not meet the purity requirements of moxa tablets, low levoborneol content, and has not been seen yet, and achieve the effects of low cost, high production efficiency, and easy operation

Inactive Publication Date: 2013-08-28
GUIZHOU LISHENGXIANG TRADITIONAL CHINESE MEDICINE SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in my country's Guizhou, Guangxi and other places, the techniques for extracting L-borneol by farmers are backward, and the extracted L-borneol content is low (the content is only about 65%), which does not meet the purity requirements of "Chinese Pharmacopoeia" for moxa tablets. Therefore, only Sold as crude L-borneol
[0004] At present, there is no report on the purification of high-purity L-borneol from the crude product L-borneol (the content of L-borneol is about 65%) sold by farmers

Method used

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  • Preparation method of high-purity levorotatory borneol
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step 1, take the commercially available crude product L-borneol (the content of L-borneol is 66.3%), centrifuge and dry it and then dry it.

[0032] Step 2, the above solid is dissolved in 2 times the amount (relative to the weight of the crude product L-borneol) in absolute ethanol.

[0033] Step 3: Add 0.02 times (relative to the weight of crude L-borneol) sodium metal in batches to the above solution under cooling conditions, and react at 0° C. for 5 hours after the addition is complete.

[0034] Step 4: Pour the above reaction solution into 4 times the amount (relative to the weight of crude L-borneol) of water, let it stand for 2 hours, and filter under reduced pressure.

[0035] Step 5, the obtained filter cake is added to 2 times the amount (relative to the weight of the crude product L-borneol) of petroleum ether, heated to 50°C, and the lower aqueous phase is separated, and the organic phase is cooled to -20°C, and a large number of flaky crystals appear. Filt...

Embodiment 2

[0037] Step 1, take the commercially available crude product L-borneol (the content of L-borneol is 66.3%), centrifuge and dry it and then dry it.

[0038] Step 2, dissolve the solid in 4 times the amount (relative to the weight of the crude product L-borneol) in absolute ethanol.

[0039] Step 3, add 0.1 times the amount (relative to the weight of crude L-borneol) of sodium metal in batches to the above solution under cooling conditions, and react at 0° C. for 2 hours after the addition is complete.

[0040] Step 4: Pour the above reaction solution into 10 times the amount (relative to the weight of crude L-borneol) of water, let it stand for 1 hour, and filter under reduced pressure.

[0041] Step 5, the obtained solid was added to 1 times the amount (relative to the weight of crude L-borneol) of petroleum ether, heated to 60°C, the lower aqueous phase was separated, and the organic phase was cooled to -5°C, a large number of crystals appeared. Filter and dry to obtain whit...

Embodiment 3

[0043] Step 1, take the commercially available crude product L-borneol (the content of L-borneol is 66.3%), and spin dry by centrifugation.

[0044] Step 2, the above solid is dissolved in 1 times the amount (relative to the weight of the crude product L-borneol) in methanol.

[0045] Step 3, adding 0.05 times the amount (relative to the weight of the crude product L-borneol) of sodium borohydride in batches to the above solution, after the addition, keep the temperature at 60°C and continue the reaction for 2 hours.

[0046] Step 4: Pour the above reaction solution into 4 times the amount (relative to the weight of crude L-borneol) of water, let it stand for 2 hours, and filter under reduced pressure.

[0047] Step 5, add the obtained solid to 1 times the amount (relative to the weight of the crude product L-borneol) of ethanol, add 0.3 times the amount (relative to the weight of the crude product L-borneol) of water, heat to 60 ° C, and all the solids are dissolved. The tem...

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Abstract

The invention belongs to the pharmaceutical field, and relates to a purifying method of levorotatory borneol. The invention discloses a preparation method of high-purity levorotatory borneol. The method comprises the following steps: performing centrifuge dripping on marketed crude levorotatory borneol (the content of levorotatory borneol is about 65%), dissolving in a reagent A, then, adding a reagent B into the liquor, and reacting for a certain time at a certain temperature; then pouring into water, standing and filtering; and recrystallizing by use of a reagent C for the filter cakes and drying to obtain the high-purity levorotatory borneol.

Description

technical field [0001] The invention belongs to the field of pharmacy, and relates to a method for purifying levoborneol, in particular to a method for preparing high-purity levoborneol. Background technique [0002] Levoborneol (also known as Levoborneol, Ai Pian, etc.) is a substance purified and processed from the Compositae plant Ainaxiang. Its efficacy is to clear the orifice, dissipate heat, improve eyesight, relieve pain, warm the middle and activate blood circulation, etc. It is mainly used to treat febrile diseases, coma, pain and phlegm confusion, suppurative otitis media, ulcerative stomatitis, burns, shingles, pharyngitis, Cardiovascular and cerebrovascular diseases and other diseases, it is a traditional Chinese medicine raw material and spice ingredient for ophthalmology, stomatology and cardiovascular medicine. Ainaxiang is mainly distributed in Guizhou, Guangxi and other places in my country. Farmers in some local areas plant a large number of Ainaxiang and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/30C07C29/74
Inventor 李知豪
Owner GUIZHOU LISHENGXIANG TRADITIONAL CHINESE MEDICINE SCI & TECH CO LTD
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