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Preparation method for ambrox

A technology of ambroxan and ambroxol, which is applied in the field of daily chemicals, can solve the problems of harsh reaction conditions, large pollution, and expensive catalysts, and achieve the effects of being suitable for industrial production, less environmental pollution, and convenient post-treatment

Active Publication Date: 2015-11-11
CHINA TOBACCO SICHUAN IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods have their own defects, or the catalyst is more expensive, or the separation and purification of the final product Ambrox is cumbersome, or the pollution is relatively large, or the reaction conditions are harsh, or because the use of low-threshold compounds such as pyridine affects Ambrox Aroma of Fragrant Ether

Method used

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  • Preparation method for ambrox
  • Preparation method for ambrox

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Experimental program
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Effect test

Embodiment

[0025] Such as figure 2 As shown, a method for preparing ambrox, in which ambroxol and activated molecular sieves are uniformly stirred and reacted in an organic solvent according to a mass ratio of 1:1 to 1:20 to obtain a reactant, and heated to reflux during the reaction 12~36 hours, obtain reactant after reaction, filter reactant after reaction, add water or organic solvent (preferably organic solvent) to filter when filtering, and reclaim molecular sieve from reactant, and filtrate (this filtrate is The solution formed by the remaining material after the molecular sieve is recovered from the reactant) is distilled and the organic solvent in the filtrate is recovered. After the filtrate is distilled, the crude product Ambroxan is obtained, and the crude product Ambroxan is obtained through recrystallization treatment. Quality Ambroxan.

[0026] The preferred mass ratio technical scheme of activated molecular sieve and organic solvent in the present invention is as follows...

Embodiment 1

[0037]Put 10g of ambroxol and 100g of 3A molecular sieve (activated at 300°C for 2 hours before use) in a 250mL three-necked flask, then add 100mL of toluene, stir evenly, heat and reflux for 20 hours, the heating temperature is 100°C, filter the reactant Molecular sieves were recovered, and the filtrate was distilled under reduced pressure to recover toluene to obtain crude ambroxan, which was dissolved in petroleum ether for recrystallization to obtain 7.71 g of white crystals. Thus the final yield of Ambrox was 83.0%.

Embodiment 2

[0039] Put 10g of Ambroxol and 100g of 4A molecular sieve (activated at 300°C for 2 hours before use) into a 250mL three-necked flask, then add 100mL of toluene, stir evenly, and heat to reflux for 20 hours at a temperature of 120°C. The reactants after the reaction were filtered to recover molecular sieves, and the filtrate was distilled under reduced pressure to recover toluene, and the crude ambrox was recrystallized with dichloromethane to obtain the target product, so that the final yield of ambrox was 78.0%.

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PUM

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Abstract

The invention discloses a preparation method for ambrox, which belongs to the technical field of daily chemicals. The preparation method employs a cheap and easily available molecular sieve as a dehydrating agent and prepares high-quality ambrox through dehydration and cyclization of the molecular sieve and diol-ambroxide in an organic solvent, wherein the molecular sieve used as the dehydrating agent can be cyclically reused. The method has the advantages of small environmental pollution, low cost, convenient post-treatment, suitability for industrial production, etc.

Description

technical field [0001] The invention relates to the technical field of daily chemicals, in particular to a method for preparing ambroxan. Background technique [0002] Ambergris is a very popular blended fragrance in the market. It is also known as the four major animal fragrances together with musk, civet, and kelp. It is famous for its strong fragrance-fixing ability and long-lasting fragrance. Natural ambergris comes mainly from the gastric acid secretions of sperm whales. Because natural ambergris is limited by resources, it is expensive and in short supply. [0003] Ambrox ((-)-Ambrox) is a precious raw material of ambergris, which has a strong and special aroma of ambergris. It is used as a substitute for natural ambergris in high-end perfumes and cosmetic essences. Because it is non-irritating to the human body and has no allergic reactions to animals, it is very suitable for perfuming skin, hair and fabrics. Ambroxan is used as an essence in cigarettes, which can ...

Claims

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Application Information

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IPC IPC(8): C07D307/92
CPCC07D307/92
Inventor 陶飞燕杨绍祥杨文敏戴亚田红玉冯广林孙宝国周胜周志刚邱光明刘如灿张艇王耀李朝荣丁为
Owner CHINA TOBACCO SICHUAN IND CO LTD
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