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Method for separating and purifying patchouli alcohol

A patchouli alcohol, separation and purification technology, applied in chemical instruments and methods, organic chemistry, bulk chemical production, etc., can solve problems such as unfavorable cost saving, unfavorable resource saving, long column chromatography period and the like, Achieving good application prospects, shortening production cycle, and simple and easy operation steps

Active Publication Date: 2014-07-30
CHENGDU HUASUN GRP INC LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If calculate by the standard of patchouli oil in " Chinese Pharmacopoeia " 2010 editions, contain patchouli alcohol in 150g patchouli volatile oil and should be more than 39g, namely the yield of patchouli alcohol in the above-mentioned column chromatography method should be lower than 20.5%, Its yield is low, which is not conducive to resource saving. At the same time, the cycle of column chromatography is long, and the solvent consumption is large, which is also not conducive to cost saving.

Method used

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  • Method for separating and purifying patchouli alcohol
  • Method for separating and purifying patchouli alcohol
  • Method for separating and purifying patchouli alcohol

Examples

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Effect test

Embodiment 1

[0045] The separation and purification method of embodiment 1 patchouli alcohol

[0046] Crush the stems and leaves of patchouli, take 2Kg, add 10 times the amount of water to soak for 2 hours, extract by steam distillation for 8 hours, collect 15g of volatile oil (mass fraction of patchouli alcohol 31.0%); use 300ml of petroleum oil to collect the volatile oil Dissolve in ether, add 2mol / L NaOH solution to extract 4 times, collect the organic solvent layer, recover the solvent under reduced pressure to obtain 10.5g of volatile oil; take the above-mentioned treated volatile oil, dissolve it with 150ml of anhydrous pyridine, cool to 0°C, add propanediol dropwise Acid monoacyl chloride 10g, after the dropwise addition, keep the temperature and stir for 4 hours, then raise the temperature to 35°C, and stir for another 2 hours; after the reaction, add 10% Na 2 CO 3 solution, stirred for 2 hours, allowed to stand for half an hour, added diethyl ether to extract twice, washed away ...

Embodiment 2

[0051] The separation and purification method of embodiment 2 patchouli alcohol

[0052] Crush the stems and leaves of patchouli, take 1.5Kg, add 10 times the amount of water to soak for 4 hours, extract with steam distillation for 10 hours, collect 12g of volatile oil (mass fraction of patchouli alcohol 32.3%); use 200ml of the collected volatile oil Dissolve petroleum ether, add 1mol / L NaOH solution to extract 5 times, collect the organic solvent layer, and recover the solvent under reduced pressure to obtain 8.7g of volatile oil; take the above-mentioned treated volatile oil, dissolve it with 120ml of anhydrous pyridine, cool to 0°C, add acetone dropwise About 8g of diacid monoacyl chloride, after the dropwise addition, keep the temperature and stir for 5 hours, then raise the temperature to 30°C, and stir for another 2 hours; after the reaction, add 12%Na 2 CO 3 solution, stirred for 2 hours, allowed to stand for half an hour, added diethyl ether to extract 3 times, washe...

Embodiment 3

[0053] The separation and purification method of embodiment 3 patchouli alcohol

[0054] Crush the stems and leaves of patchouli, take 1.0Kg, add 10 times the amount of water to soak for 2 hours, extract with steam distillation for 6 hours, collect 6.8g of volatile oil (mass fraction of patchouli alcohol 29.8%); use the collected volatile oil Dissolve 160ml of petroleum ether, add 3mol / L NaOH solution to extract 5 times, collect the organic solvent layer, and recover the solvent under reduced pressure to obtain 4.8g of volatile oil; take the above-mentioned treated volatile oil, dissolve it with 50ml of anhydrous pyridine, cool to 5°C, add dropwise Malonyl chloride is about 4g. After the dropwise addition, keep the temperature and stir for 3 hours, then raise the temperature to 30°C, and stir for another 1 hour; after the reaction, add 10% Na 2 CO 3 solution, stirred for 1 hour, allowed to stand for half an hour, added diethyl ether to extract 3 times, washed away unreacted v...

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Abstract

The invention provides a method for separating and purifying patchouli alcohol. The method includes the steps of (1) extracting volatile oil from stems and leaves of patchouli; (2) removing phenolic acid ingredients from the volatile oil to obtain phenolic acid removed volatile oil for standby; (3) subjecting the phenolic acid removed volatile oil to esterifying and salt and water extraction, and separating to obtain esterified material; (4) subjecting the esterified material obtained in the step (3) to hydrolysis reaction, extracting, and recovering solvent to obtain coarse patchouli alcohol; and (5) recrystallizing the coarse patchouli alcohol to obtain the patchouli alcohol. By the aid of the method, the patchouli alcohol with purity higher than 99% can be prepared via chemical conversion, and yield of the patchouli alcohol is higher than 40%. Compared with a conventional column chromatography method, the method is simple in operation steps, easy to operate and low in solvent consumption, can shorten production period of the patchouli alcohol, save production cost greatly, and has a good application prospect.

Description

technical field [0001] The invention relates to a method for separating and purifying patchouli alcohol. Background technique [0002] Patchouli is the dry aerial part of Pogostemon cablin (Blanco) Benth., a plant of the genus Patchouli in the Lamiaceae family. It is pungent in taste and slightly warm in nature. , published the effect of relieving heat, is an important component of various formulas and Chinese patent medicines. [0003] Patchouli oil (patchouli oil) is the main medicinal component of Patchouli. With the continuous deepening of research on pharmacological activity and chemical components, the value of volatile oils has attracted more and more attention. It has good anti-inflammatory and antibacterial activities, and Antioxidant and analgesic effects. The main components in patchouli oil are shown in the table below. [0004] [0005] Patchouli alcohol, also known as patchouli alcohol, belongs to tricyclic sesquiterpenes and is the main component of patc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C35/37C07C29/88
CPCY02P20/54
Inventor 彭成熊亮万峰唐正伟林大胜
Owner CHENGDU HUASUN GRP INC LTD
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