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Method for preparing carvone

A technology of carvone and carvone oxime, which is applied in the field of preparation of carvone, and can solve problems such as low single-step yield, complex products, and pollution

Active Publication Date: 2009-12-30
CHONGQING SHURONG CROP SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The single-step yield of this reaction is not high, and a large amount of suspected carcinogen acetone oxime and waste salt are produced, which has the problems of high cost and serious pollution
Another way is to hydrogenate carvone oxime with a poisoned catalyst, but the product is complicated, purification is difficult, and the cost of the catalyst is also high

Method used

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  • Method for preparing carvone

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preparation example Construction

[0006] The invention discloses a preparation method of carvone. Carvone oxime is oxidized by heating and refluxing with activated or fresh manganese dioxide, and the oxidation product is carvone. In this reaction, the amount of manganese dioxide used is about 1 to 15 times the molar equivalent of carvone oxime, and the required temperature is about 0°C to 100°C. The reaction formula is as follows:

[0007]

[0008] Among them, manganese dioxide can be prepared by potassium permanganate and manganese sulfate in aqueous solution. Commercially available manganese dioxide can be made into activated manganese dioxide under the action of an activator. Wherein, the activator used can be organic carboxylic acids such as acetic acid, propionic acid, butyric acid, isobutyric acid or oxalic acid, or inorganic acids such as dilute sulfuric acid, dilute hydrochloric acid, dilute phosphoric acid or dilute nitric acid. The method of activating manganese dioxide is illustrated as follow...

example 1

[0009] Example 1: Put 800g of manganese dioxide into a reaction kettle, add 2L of 5% dilute sulfuric acid, stir for 10 minutes, filter, wash with water until nearly neutral, filter and dry, and heat up to 120-125 degrees in an oven to dry 4 Hours, cooled and ground into powder form is activated manganese dioxide.

example 2

[0010] Example 2: Put 800g of manganese dioxide into the reaction kettle, add 2L of 5% dilute nitric acid, stir for 10 minutes, filter, wash with water until nearly neutral, filter and dry, and heat up to 120-125 degrees in an oven to dry 4 Hours, cooled and ground into powder form is activated manganese dioxide.

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Abstract

The invention discloses a method for preparing carvone. In the method, carvoxime is oxidized by being heated under refluxing in the presence of activated or newly prepared manganese dioxide to form an oxidation product which is the carvone.

Description

technical field [0001] The invention provides a preparation method of carvone. Background technique [0002] Carvone (also known as: 5-isopropenyl-2-methyl-2-cyclohexenyl-1-one), especially L-carvone, is used in toothpaste, tooth powder, In daily necessities such as chewing gum and mouthwash. [0003] At present, there are two main methods for preparing carvone: one is to react and hydrolyze carvone oxime with acetone under acidic conditions to obtain carvone. The single-step yield of this reaction is not high, and a large amount of suspected carcinogen acetone oxime and waste salt are produced, which has the problems of high cost and serious pollution. Another approach is to hydrogenate carvone oxime with a poisoned catalyst, but the product is complex, difficult to purify, and the cost of the catalyst is high. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a method for preparing carvone with simple steps, l...

Claims

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Application Information

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IPC IPC(8): C07C49/647C07C45/51A61K8/35
Inventor 姚文刚唐湘梅闻守军
Owner CHONGQING SHURONG CROP SCI CO LTD
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