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Method for preparing dehydrolinalyl acetate from dehydrolinalool

A technology for dehydrolinalool and linalyl ester, applied in the field of preparation of dehydrolinalyl acetate, can solve the problems of lack of industrial application value, complicated separation process, low catalyst activity, etc. The effect of ideal selectivity, short reaction time and high reactivity

Inactive Publication Date: 2008-07-02
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activity of the catalyst used in the esterification process is very low, the reaction time is as long as more than ten hours, and the process of separating the catalyst from the product is also relatively complicated, which lacks industrial application value

Method used

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  • Method for preparing dehydrolinalyl acetate from dehydrolinalool
  • Method for preparing dehydrolinalyl acetate from dehydrolinalool
  • Method for preparing dehydrolinalyl acetate from dehydrolinalool

Examples

Experimental program
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Embodiment 1~11

[0018] A 500ml three-necked flask with a stirring device is placed in a water bath, 152g of dehydrolinalool is added, nitrogen is purged for 20min, the temperature is raised to the reaction temperature with stirring, and acetic anhydride is dropped in according to the required molar ratio, and the The required amount of catalyst sulfosalicylic acid starts the reaction and is maintained for the required reaction time to complete the reaction. The product is cooled, washed with water, and statically layered to separate the oil and water phases until the oil phase material is neutral, and the oil phase material is taken to obtain the dehydrolinalyl acetate product.

[0019] The specific reaction conditions of each embodiment are shown in Table 1, and the reaction results are shown in Table 2.

[0020] Table 1.

[0021] temperature reflex

(℃)

Reaction time

(min)

The amount of catalyst

(wt%)

Raw material molar ratio

...

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Abstract

The invention relates to a method for preparing dehydrolinalyl acetate from dehydrolinalool. The method comprises esterification between dehydrolinalool and acetic anhydride is carried out in the presence of catalyst so as to obtain dehydrolinalyl acetate. Molar ratio of raw material provided of dehydrolinalool to acetic anhydride is 1: (1-5); reaction temperature is 25-70 DEG C; reaction pressure is normal pressure; reaction time is 20-150min; the catalyst is sulfosalicylic acid, dosage of which is 0.05-5wt percentage of total amount of the raw material provided. Compared with the prior art, the invention has the advantages that reaction activity of the adopted esterification catalyst is high, which is reflected by moderate reaction temperature and short reaction time, raw material conversion and product selectivity, etc. are ideal and removal of the catalyst from the product is convenient.

Description

technical field [0001] The invention relates to a preparation method of acid-containing linalyl ester, in particular to a preparation method of dehydrolinalyl acetate undergoing esterification reaction in the presence of an acidic catalyst to generate dehydrolinalyl acetate. Background technique [0002] Dehydrolinalyl acetate is an important fine chemical intermediate for the preparation of fragrances, and can be used to produce fine chemical products such as citral and ionone. Linalyl acetate can also be obtained through hydrogenation reaction of dehydrolinalyl acetate. Linalyl acetate is one of the main components of lavender oil. It has an elegant fragrance, similar to bergamot oil and lavender oil. An important raw material for spices or essences. In the prior art, linalyl acetate is mostly prepared by esterification of linalool and acetic anhydride, because linalool can be obtained from isoprene, the separated product of the C5 fraction of the by-product of petroleum ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/145
Inventor 安源郭世卓朱岳中吴卓
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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