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Synthesis of gamma-undecalactone

A synthesis method and lactone technology, applied in organic chemistry and other directions, can solve the problems of high pressure and high pressure resistance requirements of equipment, and achieve the effects of low synthesis cost, simple equipment and hindering side reactions.

Inactive Publication Date: 2009-04-08
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When this patent uses acrylic acid (water) and n-octanol to synthesize γ-undecalactone, it is carried out under the condition of high pressure and no catalyst. The pressure is high during the preparation process, and the requirements for the equipment to withstand pressure are high, and there is a certain risk.
And the technology of synthesizing gamma-undecalactone with acrylic acid under normal pressure catalyst condition has not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Add 75mL of n-octanol into a 250mL three-necked flask equipped with a balanced dropping funnel, a thermometer, and a condenser tube, weigh 0.2g of boric acid and add it to the flask, heat and stir with a magnetic stirring electric heating mantle at a speed of 500r / min, and the temperature is stable to After 170°C, start to drop a mixture consisting of 25mL of n-octanol, 2.4mL of di-tert-butyl peroxide and 8.7mL of acrylic acid at an average rate of 2.62mL / h. After the dropwise addition, keep the temperature at 170° C. and reflux for 3 hours to end the reaction. The yield was 80.53%.

Embodiment 2

[0011] Add 66mL of n-octanol to a 250mL three-necked flask equipped with a balanced dropping funnel, a thermometer, and a condenser Weigh 0.46g of zinc bromide into the flask, heat and stir with a magnetic stirring electric heating mantle at a speed of 400r / min, and after the temperature stabilizes to 170°C, start to drop 22mL of n-octanol, 1.82mL of di-tert-butyl peroxide and 5.47mL of acrylic acid, the average rate of dropping is 2.7mL / h. After the dropwise addition, keep the temperature at 170° C. and reflux for 5 h. End the reaction. The yield was 79.98%.

Embodiment 3

[0013] Add 100mL of n-octanol into a 500mL three-necked flask equipped with a balanced dropping funnel, a thermometer, and a condenser, weigh 0.7g of zinc bromide and add it to the flask, and heat and stir with a magnetic stirring electric heating mantle at a speed of 350r / min. After stabilizing to 180°C, start to drop a mixture consisting of 33mL of n-octanol, 2.1mL of di-tert-butyl peroxide and 8.9mL of acrylic acid at an average rate of 2.91mL / h. After the dropwise addition, keep the temperature at 180°C and reflux for 4h. End the reaction. The yield was 78.52%.

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Abstract

The invention discloses a method for synthesizing gamma-undecalactone, which belongs to a synthesis technology of the gamma-undecalactone. The method takes n-octanol as a solvent, boric acid or zinc bromide as a catalyst, acrylic acid as a raw material and di-t-butyl peroxide or dibenzoyl peroxide as an initiator, and comprises the following steps: firstly, adding partial n-octanol and the catalyst into a reaction kettle to be mixed and heated; secondly, mixing the remaining n-octanol, the initiator and the acrylic acid and dipping the mixture into the reaction kettle; thirdly, making the mixture react for a period; and finally obtaining reaction liquid containing the gamma-undecalactone. The method has the advantages that the reaction is carried out at normal pressure, byproducts of tert-butyl alcohol are easy to discharge from a system during the reaction process, and simultaneously the equipment used by the method is simple, the synthesis cost is low and the yield of the gamma-undecalactone is high.

Description

technical field [0001] The invention relates to a synthesis method of gamma-undecalactone, which belongs to the synthesis technology of gamma-undecalactone. Background technique [0002] γ-Undecalactone, also known as peach aldehyde, has a strong peach aroma and is naturally present in cream, osmanthus, peach, apricot, egg fruit, and hydrolyzed soybean protein. It is one of the commonly used lactone fragrances. [0003] At present, the γ-undecalactone fragrances on the market are mainly derived from chemical synthesis. There are many methods for the chemical synthesis of γ-undecalactone. The more traditional methods are the isomerization of undecylenic acid in sulfuric acid to synthesize γ-undecalactone, and the dehydration of alcohols as raw materials to generate olefins to synthesize γ-undecalactone. Lactone, using furfural as raw material to synthesize γ-undecalactone, etc. [0004] There are also many patents related to the synthesis of γ-undecalactone. Patent US56656...

Claims

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Application Information

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IPC IPC(8): C07D313/00
Inventor 许松林丁宝维
Owner TIANJIN UNIV
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