Method for preparing ambrotone

A technology of ambergris ketone and methyl group, applied in the field of synthetic perfume, can solve the problems of increasing the difficulty of washing and separation, limiting the scope of use of products, and high equipment requirements, shortening the post-reaction treatment process, improving the scope of application of products, and improving product quality. Effect

Active Publication Date: 2016-10-26
福建南平青松化工有限公司
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Problems solved by technology

[0006] Above method shortcoming is: 1, use benzene, toluene as reaction solvent, these poisonous and harmful substances are difficult to separate completely from product, have limited the scope of use of product; 2, the Diels-Alder condensation reaction of Lewis acid catalysis, because The catalyst is sensitive to water and highly corrosive, the reaction conditions are harsh, a

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  • Method for preparing ambrotone
  • Method for preparing ambrotone

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specific Embodiment approach

[0040] A method for preparing ambroxol, comprising steps ① synthesizing 3-methyl-3-penten-2 ketone, step ② diene addition to prepare ambroxone intermediate and step ③ cyclization reaction to prepare ambroxone, which It is characterized in that: Step 2. Diene addition to prepare the ambroxone intermediate is completed by high-temperature gas-phase reaction without using a catalyst.

[0041] The present invention preferably following technical scheme:

[0042] Step 2. Diene addition to prepare the ambroxone intermediate is as follows:

[0043] In reaction vessel 1, add β-pinene, then heat to 300-600°C while stirring, crack β-pinene into myrcene, and then directly introduce the cracked myrcene vapor into reaction vessel 3;

[0044] In the reaction vessel two, add the 3-methyl-3-penten-2 ketone synthesized in step ①, atomize or vaporize the 3-methyl-3-penten-2 ketone, and then atomize or vaporize the 3-Methyl-3-penten-2-ketone is introduced into the reaction vessel three, so tha...

Embodiment 1- Embodiment 4

[0065] Embodiment 1-embodiment 4 is the specific example of synthesizing 3-methyl-3-penten-2 ketone

Embodiment 1

[0067] In a 250mL glass jacketed reaction kettle equipped with a reflux condenser, mechanical stirring, thermometer and dropping funnel, butanone (60.0g, 0.833mol) and potassium hydroxide (1.50g, 0.0270mol) were added successively, and the reaction kettle After the temperature was slowly heated to 40°C, 40% acetaldehyde aqueous solution (83.3g, 0.758mol) was added dropwise at this temperature, and the reaction temperature was controlled between 40-45°C. After the dropwise addition, the reaction was carried out at constant temperature for 3 h. After the chromatographic detection reaction was completed, 40 g of ice water was slowly added to the reaction kettle, and neutralized to neutral with concentrated hydrochloric acid. After stirring at room temperature for 30 minutes, the layers were separated. The organic phase was rectified under reduced pressure, and the 68°C / 50mmHg fraction was collected to obtain light yellow liquid compound III (61.1 g, 0.623 mol), with a yield of 9...

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Abstract

The invention relates to a method for preparing ambrotone. The method includes steps of 1, synthesizing 3-methyl-3-pentene-2-ketone; 2, carrying out diene addition for preparing ambrotone intermediates; 3, carrying out cyclization reaction to prepare the ambrotone. Diene addition for preparing the ambrotone intermediates is carried out without catalysts by the aid of high-temperature gas-phase reaction. The method has the advantages that the ambrotone is prepared from raw materials beta-pinene, butanone and acetaldehyde, other organic solvents are omitted, high-pollution and high-carcinogenesis substances such as benzene and toluene are omitted, accordingly, the cost can be lowered, the quality of products can be effectively improved, the application range of the products can be effectively expanded, and Diels-Alder condensation reaction is carried out by the aid of the high-temperature gas-phase reaction; the Diels-Alder condensation reaction is carried out by the aid of the high-temperature gas-phase reaction or atomized small-molecule water drop and gas phases, catalysts such as Lewis acid or proton acid are omitted at reaction steps, accordingly, the production cost can be lowered, technological equipment can be simplified, post-reaction treatment working procedures can be shortened, and the purpose of zero sewage discharge can be truly achieved.

Description

technical field [0001] The invention belongs to the technical field of synthetic perfumes, in particular to a method for preparing ambroxol by only using β-pinene, methyl ethyl ketone and acetaldehyde. Background technique [0002] Ambroxone, colorless or light yellow liquid, has a woody, amber-like aroma. Its molecular formula is C 16 h 26 O, is a mixture of 2,3,8,8-tetramethyl-2-acetyloctahydronaphthalene. Due to the similar smell and effect of ambergris, it is widely used in various fields. At present, ambroxol is mainly used in: deodorant, refreshing fragrance, perfume essence blending agent and tobacco industry, etc. [0003] At present, spice companies in many countries are conducting research on the synthesis of ambroxone. In 1975, the American International Fragrance Company applied for a patent for the three-step synthesis of ambroxone. Its chemical reaction formula (1) is as follows, and must add catalyzer when this method prepares ambroxone, does not add cat...

Claims

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Application Information

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IPC IPC(8): C07C49/553C07C45/67C07C49/557
CPCC07C45/67C07C45/74C07C49/553C07C49/557C07C49/203
Inventor 华建军郑飞剑沈裕斌谢鹏辉
Owner 福建南平青松化工有限公司
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