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Method for synthesizing high-purity borneol

A high-purity, borneol technology, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of hydroxyl compounds, etc., can solve the problems of high price, low product yield, high production cost, etc., and save reaction time , The preparation method is simple, the effect of reducing the cost of raw materials

Inactive Publication Date: 2019-07-16
WUZHOU HUANGPU CHEM PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, natural borneol resources are very limited and expensive, which is far from meeting the increasing needs of human beings. It is an inevitable trend of development to replace natural borneol with synthetic borneol.
[0004] When the existing method synthesizes borneol, there are disadvantages such as cumbersome catalyst preparation process, complicated process, long time consumption, high production cost, low yield in the product, and low selectivity of borneol.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Raw material preparation

[0023] 1.1 Preparation of α-pinene:

[0024] Pump 4,000-5,000 kg of turpentine into the turpentine-pinene fractionation kettle. The outlet of the pump is provided with a flowmeter interlock cut-off valve to ensure that the amount of turpentine pumped into the turpentine fractionation tower is a certain value. The temperature of the kettle rises to 90-125°C, and the pressure difference between the top of the tower and the bottom of the tower is kept at 12KPa by controlling the amount of heat transfer oil. When the temperature of the top of the tower rises to >60°C, open the water valve of the condenser on the top of the tower. When distillate is observed in the discharge flowmeter (or sight glass), close the discharge flowmeter and its bypass valve, and fully reflux for 20 to 30 minutes. After the total reflux is stable, adjust the discharge volume to 300L / h, and the previous distillation receiving tank accepts the previous fraction, and inter...

Embodiment 2

[0032] The difference from Example 1 is that 300Kg α-pinene is put into the reaction pot, and the stirring is started. Balance the internal and external temperatures, and control the internal temperature below 40°C for feeding. Put 82Kg of anhydrous oxalic acid and 12Kg of hydrated titanium dioxide into the reaction pot after being filtered through a funnel with a 20-mesh screen. Observe the change of internal temperature at any time during feeding. If the temperature rises rapidly (more than 1°C in 1 minute), stop feeding immediately, and turn on cooling water for cooling control. The feeding can only be continued when the internal temperature drops below 40°C. Carry out esterification reaction then, the first stage reaction temperature is 50 ℃, and reaction time is 4 hours; The second stage reaction temperature is 75 ℃, and reaction time is 1 hour, and the third stage reaction temperature is 88 ℃, reaction 1 hour. After the reaction is completed, filter and recover the cata...

Embodiment 3

[0034] The difference from Example 1 is that 300Kg α-pinene is put into the reaction pot, and the stirring is started. Balance the internal and external temperatures, and control the internal temperature below 40°C for feeding. Put 82Kg of anhydrous oxalic acid and 12Kg of hydrated titanium dioxide into the reaction pot after being filtered through a funnel with a 20-mesh screen. Observe the change of internal temperature at any time during feeding. If the temperature rises rapidly (more than 1°C in 1 minute), stop feeding immediately, and turn on cooling water for cooling control. The feeding can only be continued when the internal temperature drops below 40°C. Carry out esterification reaction then, the first stage reaction temperature is 55 ℃, and reaction time is 3 hours; The second stage reaction temperature is 75 ℃, and reaction time is 1 hour, and the third stage reaction temperature is 88 ℃, reaction 1 hour. After the reaction is completed, filter and recover the cata...

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PUM

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Abstract

The invention discloses a method for synthesizing high-purity borneol, relates to the field of borneol synthesis, and aims to provide a borneol synthesis method with low manufacturing cost, short reaction time and high purity. The synthesis method comprises the following steps: carrying out an esterification reaction on alpha-pinene with anhydrous oxalic acid under the action of a catalyst to obtain bornyl oxalate, carrying out a saponification reaction on the bornyl oxalate to obtain crude borneol, and then carrying out crystallizing for 2-4 times. The esterification reaction comprises threereaction stages, wherein the reaction temperature in a first stage is 45-65 DEG C, the reaction temperature in a second stage is 65-75 DEG C, and the reaction temperature in a third stage is 75-88 DEGC. The high-purity borneol is used for antibacterial and anti-inflammatory drugs.

Description

technical field [0001] The present invention relates to the preparation of borneol, in particular to a method for synthesizing high-purity borneol. Background technique [0002] Borneolum, whose English name is Borneolum Syntheticum, is a colorless transparent or white translucent flaky crisp crystal; it is fragrant, pungent and cool; it is volatile, and when ignited, it produces thick smoke and a bright flame. Borneolum has significant effects in many aspects such as antibacterial, anti-inflammatory, analgesic, anti-fertility, etc. Many famous and valuable Chinese patent medicines use it as one of the main components of drugs, such as Bingboran Powder, Niuhuang Jiedu Pills, Angong Niuhuang Pills, and Calculus Bezoar Shangqing pills, Suhexiang pills, etc. [0003] There are two epimers of borneol and isoborneol, but it is generally believed in medicine that the side effects of isoborneol are much greater than that of borneol. Therefore, the price of orthoborneol is much mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/30C07C27/02C07C29/78C07C69/36C07C67/08
CPCC07C29/095C07C29/78C07C67/08C07C2602/42C07C69/36C07C35/30
Inventor 周建华廖恒安陈小宝
Owner WUZHOU HUANGPU CHEM PHARM CO LTD
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