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Method for synthesizing vanillin ester isobutyric acid through method of acid anhydride

A technology of vanillin isobutyrate and acid anhydride is applied in the field of synthesis of spice vanillin isobutyrate, can solve the problems of complex process of vanillin isobutyrate, low product yield and the like, and achieves the product yield. High efficiency, simple process and few by-products

Inactive Publication Date: 2006-07-05
上海香料研究所
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Problems solved by technology

The vanillin isobutyrate obtained by the usual method is complex and the product yield is low

Method used

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  • Method for synthesizing vanillin ester isobutyric acid through method of acid anhydride

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Embodiment Construction

[0008] Further illustrate the implementation of the present invention below:

[0009] The preparation of vanillin isobutyrate: add toluene 115ml, 106.5 grams (0.70mol) vanillin, 5.3 grams (0.05mol) carbonic acid Sodium, turn on stirring. At room temperature, which may be 25 degrees Celsius, 129.3 grams (0.78 mol) of isobutyric anhydride was added dropwise, and the addition was completed in about 1 hour, and then continued to stir for 2 hours. Stirring was stopped and washed with 15% sodium hydroxide solution and then with water. The solvent was recovered, and then 154.3 grams of product were obtained by distillation under reduced pressure, with a content of 99.1%, and a yield of 99.2%.

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Abstract

This invention publishes a synthesis method for vanillin isobutyrate. Toluene, vanillin and sodium carbonate are added in turn into a three-neck flask which is equipped with a stirrer, a dropping funnel and an inner thermometer and the stirrer is then turned on; isobutanoic anhydride is dropped into the flask at room temperature in 1 hour and the whole system is then stirred for 2 more hours; stop stir; the mixture is washed with a 15% sodium hydroxide solution and water in turn; the solvent is recycled and the mixture is vacuum distilled to obtain vanillin isobutyrate. This invention has the advantages of room-temperature reaction, little byproduct, simple purification technique and a high yield.

Description

technical field [0001] The invention relates to a method for synthesizing spice vanillin isobutyrate. Background technique [0002] Vanillin isobutyrate has a strong, sweet, creamy aroma, vanilla-nutmeg flavor, used in baked goods, soft candy, jelly and pudding, chewing gum, etc. The vanillin isobutyrate obtained by the usual method is complex and the product yield is low. Contents of the invention [0003] Aiming at the shortcomings of the prior art, the invention provides an improved synthesis method of vanillin isobutyrate, and obtains vanillin isobutyrate with a higher yield. [0004] Using sodium carbonate as a catalyst, at room temperature, vanillin is reacted with isobutyric anhydride to obtain vanillin isobutyrate. [0005] It reacts as follows: [0006] [0007] The invention has the advantages of simple process, less by-products and high product yield. detailed description: [0008] Further illustrate the implementation of the present invention below: ...

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Application Information

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IPC IPC(8): C07C69/035C07C67/08
Inventor 周治国
Owner 上海香料研究所
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