Preparation method of ambrotone

A technology for obtaining ambroxone and butanone, which is applied in the preparation field of ambroxone, can solve the problems of aluminum trichloride being difficult to wash, the color of ambroxone is yellow, and the production cost is increased, and the reaction temperature can be easily controlled, The effect of obvious layering and cost saving

Active Publication Date: 2015-05-20
ANHUI SANHUAN PAPER GRP
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation method of ambroxone uses a large amount of strong acid added in the condensation reaction, which increases the production cost. However, toluene and aluminum chloride are used as catalysts in the addition reaction, which causes large pollution, and the loss of reclaiming toluene is large, and the trichloride Aluminum is not easy to clean and is highly corrosive to equipment
In the third step cyclization reaction, the amount of reaction acid used is large, and the color of ambroxone produced is yellow

Method used

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Examples

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Embodiment Construction

[0018] The technical solution of the present invention will be further explained and illustrated through specific implementation methods below.

[0019] The raw materials used in the following examples are all commercially available products, and the rectifying equipment is a kettle with a model of 5 tons and 10 tons. The manufacturer: Zibo Changshun Chemical Equipment Factory

[0020] The preparation of ambroxone comprises the steps:

[0021] (1) Condensation reaction

[0022] Take butanone to prepare 356 kg of a mixture containing 6-8% water, add it to the reactor, and add 75 kg of hydrochloric acid solution with a concentration of 32% to the reactor at the same time, after stirring evenly, add 145-150 kg of acetaldehyde dropwise at a rate of 50 kg per hour; Control the temperature at 35-40°C; when the drop is finished, keep it warm at 50-60°C for 1 hour to obtain the reaction product; cool the reaction product to 25°C, neutralize the pH to 8-10 with 20% sodium hydroxide by...

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Abstract

The invention discloses a preparation method of ambrotone. The method is characterized by comprising the following steps of: performing a condensation reaction, an addition reaction, a cyclization reaction and the like, wherein during the condensation reaction, butanone and acetaldehyde react in a hydrochloric acid solution at the temperature of 35 to 40 DEG C, thereby obtaining 3-methyl-3-pentene-2-ketone as an intermediate product; the addition reaction is carried out between the intermediate product and acetic anhydride under the catalytic condition of a boron trifluoride catalyst, thereby obtaining cyclic ketone; and the cyclization reaction is carried out on the cyclic ketone, thereby obtaining the ambrotone as a final product. During the condensation reaction, the usage amount of the hydrochloric acid is reduced greatly, so that the cost is lowered; and the content of the rectified 3-methyl-3-pentene-2-ketone is improved to 98%. During the cyclization reaction, the temperature is controlled between 60 and 65 DEG C, so that the odor of the obtained final product is changed greatly, i.e., the ambrotone fragrance is increased while the elecampane is weakened; and the ambrotone fragrance is easily accepted by a consumer. In addition, the ambrotone is faint yellow in color, so that the color luster is soft. The method is low in production cost and environmental-friendly, and the purity and yield of the obtained product are further improved.

Description

technical field [0001] The invention relates to a method for preparing spices, in particular to a method for preparing ambroxone. Background technique [0002] Ambergris is a colorless to pale yellow liquid, a synthetic amber fragrance. Its aroma is similar to that of natural ambergris and amber, and is extremely long-lasting. It is mostly used in the essence of cologne, soap and detergent. At present, the preparation method of ambroxone uses a large amount of strong acid added in the condensation reaction, which increases the production cost. However, toluene and aluminum chloride are used as catalysts in the addition reaction, which causes large pollution, and the loss of reclaiming toluene is large, and the trichloride Aluminum is not easy to clean, and it is highly corrosive to equipment. In the third step cyclization reaction, the use amount of reaction acid is large, and the color of the ambroxone produced is yellow. Contents of the invention [0003] In order to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/553C07C45/67
Inventor 华洪生严加友
Owner ANHUI SANHUAN PAPER GRP
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