Production technology of sclareolide synthesized from sclareol

A technology of sclareolide and sclareolide, applied in the direction of organic chemistry and the like, can solve the problems of low conversion rate, long reaction time, unsuitable for industrial production and the like, and achieve the effect of improving the conversion rate and shortening the reaction time

Inactive Publication Date: 2012-11-07
JIAOZUO XINZHIYUAN TECH
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  • Application Information

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Problems solved by technology

Chinese patent, patent number: 2005100417218, published on February 24, 2005, discloses a synthetic method of sclareolide, which uses sclareol as raw material, hydrogen peroxide as oxidant, and contains VIB group transition metal elements The compound is

Method used

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Experimental program
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Effect test

Embodiment 1

[0014] Follow the steps below to synthesize sclareolide:

[0015] a, cracking section, add 30% acetic acid solution 190L, hydrogen peroxide composite oxidant 90L, heteropolyacid salt catalyst 0.4kg, tetrabutylammonium bromide 2kg, sclareol 6kg in the cracking kettle, heat up to 90 ℃, The reaction solution was passed into ozone gas at a rate of 10 L / min, cooled after 4 hours of reaction, the reaction solution was transferred to a receiving tank, 200 L of toluene was added, stirred for extraction;

[0016] b. In the hydrolysis section, pump the upper organic phase in the receiving tank into the hydrolysis tank, then add 4kg of tetrabutylammonium bromide and 15kg of 1% potassium hydroxide solution, raise the temperature to 90°C, keep it for 3 hours, then add 1000L of water to stir, stand still;

[0017] c, acidification section, put the lower water phase in the hydrolysis tank into the neutralization tank, adjust the pH to 3 with sulfuric acid solution, let it stand, and then ca...

Embodiment 2

[0021] Follow the steps below to synthesize sclareolide:

[0022] a, cracking section, add 30% acetic acid solution 200L, hydrogen peroxide composite oxidant 100L, heteropolyacid salt catalyst 0.5kg, tetrabutylammonium bromide 5kg, sclareol 6kg in the cracking kettle, heat up to 90 ℃, The reaction solution was passed into ozone gas at a rate of 10 L / min, cooled after 4 hours of reaction, the reaction solution was transferred to a receiving tank, 200 L of toluene was added, stirred for extraction;

[0023] b. In the hydrolysis section, the upper organic phase in the receiver tank is pumped into the hydrolysis tank, then 5 kg of tetrabutylammonium bromide and 20 kg of 1% potassium hydroxide solution are added, the temperature is raised to 90 ° C, and maintained for 3 hours, then 1000 L of water is added to stir, stand still;

[0024] c, acidification section, put the lower water phase in the hydrolysis tank into the neutralization tank, adjust the pH to 3 with sulfuric acid sol...

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PUM

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Abstract

The invention discloses a production technology of sclareolide synthesized from sclareol. The technology successively comprises the following steps of: cracking station, hydrolysis station, acidifying station, ring closing station and purification so as to obtain 95% of sclareolide. An oxidizing agent used in the method is a hydrogen peroxide composite oxidizing agent and a catalyst is heteropolyacid salt. The invention has the following beneficial effects: by the use of the composite oxidizing agent and the catalyst heteropolyacid salt for reaction instead of using a hydrogen peroxide single oxidizing agent, conversion rate is raised by 22-25%, reaction time is greatly shortened, and the reaction time is reduced from more than 20 hours to less than 10 hours.

Description

technical field [0001] The invention relates to a production process of sclareolide, in particular to a production process for synthesizing sclareolide from sclareol. Background technique [0002] Sclareolide is an important ambergris-type synthetic fragrance. [0003] Sclareolide is usually synthesized from sclareol, and the key is to oxidize and degrade the side chain of sclareol. Chinese patent, patent number: 2005100417218, published on February 24, 2005, discloses a synthetic method of sclareolide, which uses sclareol as raw material, hydrogen peroxide as oxidant, and contains VIB group transition metal elements The compound is used as a catalyst, and the reaction is carried out in a water-organic solvent mixture to synthesize sclareolide. This method has low cost and no environmental pollution, but the conversion rate is not high and the reaction time is long, so it is not suitable for industrial production. Contents of the invention [0004] Aiming at the problems...

Claims

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Application Information

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IPC IPC(8): C07D307/92
Inventor 李云政赵俊岩张春辉赵新岩
Owner JIAOZUO XINZHIYUAN TECH
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