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(1S,4aS,8aS)-Decahydro-5,5,8a-trimethyl-2-methylene-1-naphthaleneacetaldehyde-based spice and preparation process thereof

A technology of ambroxone and spices, which is applied in the field of spice processing, can solve the problems of environmental pollution, long time consumption, and reduce the production efficiency of ambroxone spices, so as to improve the production efficiency and prevent environmental pollution.

Inactive Publication Date: 2020-10-30
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing preparation process of ambroxol fragrance takes a long time, and phosphoric acid is used as a catalyst in the synthesis of ambroxone. The use of phosphoric acid catalyst will cause great pollution to the environment, and the catalytic efficiency is low, which greatly reduces the Preparation Efficiency of Ambroxol Flavor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A fragrance based on ambroxol, made by the following steps:

[0030] Step S1: Add methyl ethyl ketone and ethanol into the stirred tank, and stir at a rotation speed of 60r / min and a temperature of 10°C until the methyl ethyl ketone is completely dissolved, and then add potassium hydroxide dropwise at a temperature of 5°C solution, dropwise for 5 minutes, after the dropwise addition, add acetaldehyde dropwise, dropwise for 1 hour, continue to stir for 3 minutes, raise the temperature at 30°C, and react for 3 hours, then add glacial acetic acid to the pH value of the reactant 7, after standing still to divide the water, the temperature was raised to 80°C for distillation to remove ethanol to obtain 3-methyl-3-penten-2-one;

[0031] Step S2: Add the 3-methyl-3-penten-2-one and myrcene prepared in step S1 into the reaction kettle, and stir for 5 minutes under the conditions of rotation speed of 200r / min and temperature of 15°C, Add tetrahydrofuran and p-toluenesulfonic ac...

Embodiment 2

[0038] A fragrance based on ambroxol, made by the following steps:

[0039] Step S1: Add methyl ethyl ketone and ethanol into the stirred tank, and stir at a rotation speed of 70r / min and a temperature of 13°C until the methyl ethyl ketone is completely dissolved, and then add potassium hydroxide dropwise at a temperature of 8°C Solution, dropwise time 8min, after dropwise addition, dropwise add acetaldehyde, dropwise time is 1.3h, continue to stir for 4min, heat up under the condition of 33°C, react for 3.5h, add glacial acetic acid to the reactant The pH value is 7. After standing still to separate the water, the temperature is raised to 83°C for distillation to remove ethanol to obtain 3-methyl-3-penten-2-one;

[0040] Step S2: Add the 3-methyl-3-penten-2-one and myrcene prepared in step S1 into the reaction kettle, and stir for 8 minutes under the conditions of rotation speed of 250r / min and temperature of 18°C, Add tetrahydrofuran and p-toluenesulfonic acid, react for 5....

Embodiment 3

[0047] A fragrance based on ambroxol, made by the following steps:

[0048] Step S1: Add methyl ethyl ketone and ethanol into the stirred tank, and stir at a rotation speed of 80r / min and a temperature of 15°C until the methyl ethyl ketone is completely dissolved, and then add potassium hydroxide dropwise at a temperature of 10°C solution, dropwise for 10min, after the dropwise addition, dropwise add acetaldehyde, dropwisely for 1.5h, continue to stir for 5min, raise the temperature at 35°C, react for 4h, then add glacial acetic acid to the pH of the reactant The value is 7. After standing still to separate the water, the temperature is raised to 85°C to carry out distillation to remove ethanol to obtain 3-methyl-3-penten-2-one;

[0049] Step S2: Add the 3-methyl-3-penten-2-one and myrcene prepared in Step S1 into the reaction kettle, and stir for 10 minutes under the conditions of a rotation speed of 300 r / min and a temperature of 20°C, Add tetrahydrofuran and p-toluenesulfo...

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PUM

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Abstract

The invention discloses a (1S,4aS,8aS)-Decahydro-5,5,8a-trimethyl-2-methylene-1-naphthaleneacetaldehyde-based spice and a preparation process thereof. According to the method, butanone and acetaldehyde are used as raw materials for aldehyde ketone condensation; then, myrcene and 3-methyl-3-pentene-2-one are used for carrying out diene addition; and finally, a diene addition product is cyclizedto obtain the product. A catalyst is prepared in the cyclization process; the catalyst is prepared by the following steps: polymerizing a styrene micromonomer to prepare a first matrix; sulfonating the first matrix under the action of sulfuric acid to obtain a second matrix; and soaking the second matrix in a ferric chloride solution to produce the catalyst. The catalyst is a cation exchange resincatalyst, compared with the prior art, phosphoric acid is not used for catalysis, environmental pollution is prevented, metal iron ions are loaded on the cation exchange resin, sulfonic acid acid acid groups on the surface of the catalyst can be combined with the iron ions through complexation, then a stronger acid center is formed, and the preparation efficiency of the (1S,4aS,8aS)-Decahydro-5,5,8a-trimethyl-2-methylene-1-naphthaleneacetaldehyde is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of spice processing, and in particular relates to an ambroxone-based spice and a preparation process thereof. Background technique [0002] The chemical name of ambroxone is: 2-acetyl-1, 2, 3, 4, 5, 6, 7, 8-octahydro-2, 3, 7, 8-tetramethylnaphthalene, which is several isomers It has both woody and ambergris, long-lasting aroma and stable properties, and can be used as a spice or a fixative. The current common synthetic route of ambergris is the following three steps, first synthesizing 3-methyl- 3-penten-2-one, and then use myrcene, 3-methyl-3-penten-2-one for diene addition, and finally use the product of diene addition for cyclization in the system. [0003] The existing preparation process of ambroxol fragrance takes a long time, and phosphoric acid is used as a catalyst in the synthesis of ambroxone. The use of phosphoric acid catalyst will cause great pollution to the environment, and the catalytic eff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/74C07C45/68C07C45/67C07C49/203C11B9/00C11B9/02B01J31/22
CPCB01J31/226B01J2231/52B01J2531/842C07C45/673C07C45/68C07C45/74C11B9/0053C11B9/022C07C2602/28C07C49/203
Inventor 王天义范一义汪洋徐基平张政徐基龙董金龙
Owner ANHUI HYEA AROMAS
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