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Method for preparing cinnamyl acetate

A technology of cinnamyl acetate and cinnamyl alcohol, which is applied in the chemical field, can solve the problems of product purity failing to meet quality standards, long production cycle, complicated process, etc., and achieve stable and reliable product quality, low production cost, and easy-to-obtain raw materials

Inactive Publication Date: 2008-09-10
湖北远成赛创科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The general method of preparing cinnamyl acetate mainly contains at present: 1, adopt hot caustic alkali solution to process natural styrax balsam, white Peru balsam, cinnamon oil, silver white acacia oil to extract cinnamyl acetate, and this method produces and prepares cinnamyl acetate The cost is high, raw materials are hard to find, the process is complicated, the production cycle is long, and the environment is seriously polluted; 2. It is produced by the direct esterification reaction of cinnamyl alcohol and acetic acid in the presence of concentrated sulfuric acid. Although the process of producing cinnamyl acetate by this method is simple , but many by-products, poor product purity, low yield; 3, by cinnamyl alcohol and acetic anhydride directly prepare cinnamyl acetate through acetylation reaction, this technique is simple, easy to operate, but the transformation rate of raw material cinnamyl alcohol used is low, Product purity does not reach the quality standard; 4, adopt sodium acetate and cinnamyl chloride to react in the presence of N,N-dimethylformamide to prepare cinnamyl acetate, the raw material cinnamyl chloride used in this process is poisonous and expensive, and the market supply is limited , the used solvent N, the N-dimethylformamide price is also relatively expensive, and the product yield has only 54%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Dissolve 0.7g 85% phosphoric acid or p-toluenesulfonic acid in 150g (1.47mol) acetic anhydride and stir evenly, keep the temperature at 20 or 24 or 28 or 32 or 37 or 42 or 45°C and add 134g (1.0mol) of cinnamyl alcohol dropwise, Alcohol dripping time is 5 or 6 or 7 hours. The cinnamyl alcohol is added dropwise and kept at 40 or 44 or 48 or 50° C. for 1 or 2 hours. After the heat preservation is completed, the crude product of cinnamyl acetate is obtained by washing with water and neutralizing. The obtained cinnamyl acetate was collected at 170-174° C. under the condition of reduced pressure -0.096Mpa, 143.4 g of cinnamyl acetate was finished, and the yield was 82.4%. The product purity reaches 98.4%.

Embodiment 2

[0013] Dissolve 1.4g of 88% phosphoric acid or p-toluenesulfonic acid in 102g (1.0mol) of acetic anhydride and stir evenly, keep the temperature at 20 or 22 or 26 or 30 or 35 or 40 or 45°C and add 134g (1.0mol) of cinnamyl alcohol dropwise. Alcohol dripping time is 5 or 6 or 7 hours. The cinnamyl alcohol is added dropwise and kept at 40 or 43 or 47 or 50° C. for 1 or 2 hours. After the heat preservation is completed, the crude product of cinnamyl acetate is obtained by washing with water and neutralizing. The obtained cinnamyl acetate was collected at 162-166° C. under the condition of reduced pressure -0.098Mpa, 148.0 g of cinnamyl acetate finished product, yield 84.1%. The product purity reaches 98.5%.

Embodiment 3

[0015] Dissolve 2.7g of 92% phosphoric acid or p-toluenesulfonic acid in 204g (2mol) of acetic anhydride and stir evenly, keep the temperature at 20 or 23 or 27 or 31 or 39 or 43 or 45°C and add 134g (1.0mol) of cinnamyl alcohol dropwise. The dropping time is 5 or 6 or 7 hours. The cinnamyl alcohol is added dropwise and kept at 40 or 45 or 49 or 50° C. for 1 or 2 hours. After the heat preservation is completed, the crude product of cinnamyl acetate is obtained by washing with water and neutralizing. The obtained cinnamyl acetate was collected at 154-157° C. under the condition of reduced pressure -0.099Mpa, 151.7 g of cinnamyl acetate finished product, yield 86.2%. The product purity reaches 98.5%.

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Abstract

The invention discloses a preparation method for cinnamyl acetate. The steps of the method are as follows: A) cinnamic alcohols and acetic anhydrides are mixed for reaction according to a certain mol ratio; catalysts are taken to dissolve in the acetic anhydrides, and the temperature is preserved, and the cinnamic alcohols are dropwise added; B) after the addition of the cinnamic alcohols, the temperature is kept in the range of from 40 to 50 DEG C for reaction; C) after the heat preservation, the cinnamyl acetate products are obtained by the water washing and neutralization; D) the cinnamyl acetate products obtained undergo the fraction collection under the vacuum of negative 0.096 to negative 0.1Mpa, obtaining the cinnamyl acetate finished products; the invention has the advantages of simple method, convenient operation, low material costs, high yield and no environmental pollution, and is quite suitable for the industrialized production; moreover, the yield of the production of the cinnamyl acetate is as high as 88.6 percent.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a preparation method of cinnamyl acetate, which is mainly used as spices to configure cinnamon, apple, cherry and pineapple flavors; used as hyacinth, clove, lily of the valley, jasmine, mast and other flavors blend of spices. Background technique [0002] The chemical name of cinnamyl acetate is phenylpropenyl acetate, which is an important fine chemical intermediate widely used in the production of medicines, spices and other products. The general method of preparing cinnamyl acetate mainly contains at present: 1, adopt hot caustic alkali solution to process natural styrax balsam, white Peru balsam, cinnamon oil, silver white acacia oil to extract cinnamyl acetate, and this method produces and prepares cinnamyl acetate The cost is high, the raw materials are hard to find, the process is complicated, the production cycle is long, and the environment is seriously polluted; 2...

Claims

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Application Information

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IPC IPC(8): C07C69/145C07C67/08
Inventor 叶传发朱如慧余苗苗阮令飞华好好
Owner 湖北远成赛创科技有限公司
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