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Method for compounding allyl amyl glycolate

A synthesis method and the technology of Gapon ester are applied in the field of preparation of daily chemical fragrances, which can solve the problems of complicated process and complicated raw materials, and achieve the effects of environmental safety and friendliness, easy operation and mild reaction conditions.

Inactive Publication Date: 2010-06-09
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The raw materials used in this method are complicated and the process is relatively complicated.

Method used

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  • Method for compounding allyl amyl glycolate

Examples

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Effect test

Embodiment 1

[0027] The first step, the preparation of isoamyloxyacetic acid

[0028] In a 500 ml three-necked flask equipped with a stirrer, a thermometer, and a fractionating column, add 15 grams (0.22 mol) of sodium ethoxide and 290 grams of isoamyl alcohol (3.3 mol), stir, start heating, and slowly distill the alcohol to the top. Warm at 125°C to obtain sodium isoamyloxide solution. Cool to an internal temperature of 60-80°C, start adding 0.25 mol of chloroacetic acid, and continue to react for 2 hours at an internal temperature of 65°C. Then, it was heated to an internal temperature of 130° C. to recover isoamyl alcohol. Finally, 200 ml of water was added and steam distillation was performed to remove residual isoamyl alcohol. After the reaction solution was cooled, add 20% hydrochloric acid to acidify, separate the organic layer, wash with water, dry, and collect the fraction at 116-118°C / 5mmHg by distillation under reduced pressure to obtain 13.9 grams of isopentyloxyacetic acid (...

Embodiment 2

[0032] The first step, the preparation of isoamyloxyacetic acid

[0033] In a 500 ml three-necked flask equipped with a stirrer, a thermometer, and a fractionating column, add 15 grams (0.22 mol) of sodium ethoxide and 290 grams of isoamyl alcohol (3.3 mol), stir, start heating, and slowly distill the alcohol to the top. Warm at 125°C to obtain sodium isoamyloxide solution. Cool to an internal temperature of 65°C, add 9.5 g (0.1 mol) of chloroacetic acid, and continue the reaction at an internal temperature of 60°C for 2 hours. Then, it is heated to an internal temperature of 135° C. to recover isoamyl alcohol. Finally, 200 ml of water was added and steam distillation was performed to remove residual isoamyl alcohol. After the reaction solution was cooled, add 52.8 grams of 20% hydrochloric acid to acidify it, separate the organic layer, wash with water and dry it, and collect the fraction at 116-118°C / 5mmHg by distillation under reduced pressure to obtain 13.8 grams (95.4%)...

Embodiment approach 3

[0037] The first step, the preparation of isoamyloxyacetic acid

[0038] In a 500 ml three-necked flask equipped with a stirrer, a thermometer, and a fractionating column, add 15 grams (0.22 mol) of sodium ethoxide and 290 grams of isoamyl alcohol (3.3 mol), stir, start heating, and slowly distill the alcohol to the top. Warm at 125°C to obtain sodium isoamyloxide solution. Cool to an internal temperature of 60°C, add 18.9 g (0.2 mol) of chloroacetic acid, and continue the reaction at an internal temperature of 60°C for 1 hour. Then, it was heated to an internal temperature of 130° C. to recover isoamyl alcohol. Finally, 200 ml of water was added and steam distillation was performed to remove residual isoamyl alcohol. After the reaction solution was cooled, add 105.6 grams of 20% hydrochloric acid to acidify it, separate the organic layer, wash with water and dry it, then collect the fraction at 116-118°C / 5mmHg by distillation under reduced pressure to obtain 25.9 grams (96....

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Abstract

The invention discloses a method for preparing daily chemical spice, in particular to a method for compounding allyl amyl glycolate. The allyl amyl glycolate is generated by two steps of reaction, in the first step, isoamylol and sodium ethylate carry out alcohol exchange to prepare sodium isoamylol, and the sodium isoamylol and chloroacetic acid remove sodium chloride to compound isopentyloxy acetic acid; and in the second step, the isopentyloxy acetic acid and allyl alcohol are esterified under the existence of acid catalyst to prepare the allyl amyl glycolate. The invention has the advantages of improvement of traditional method of isopentyloxy acetic acid, easy acquisition of adopted raw materials, mild reaction condition, safer and more friend process and high yield, and the product has strong fruit odour which is galbanum odour slightly with pineapple odour. The allyl amyl glycolate is widely applied to daily odour adding products, such as detergent, fabric softener, bath cream, and the like and endows essence with modern flavor.

Description

technical field [0001] The invention relates to a preparation method of daily chemical fragrance, in particular to a synthesis method of glycopyrrolate. technical background [0002] Gepong esters have a strong fruity aroma with a hint of pineapple-like Gepong. Widely used in detergents, fabric softeners, shower gels and other daily fragrance products, giving the fragrance a modern flavor. [0003] Its chemical name is: allyl isopentyloxyacetate. The synthetic method of present common glycopyrrolate is as follows: [0004] Method 1: First prepare sodium isoamyloxide by reacting metal sodium and isoamyl alcohol, then react with chloroacetic acid, and dechlorinate sodium to synthesize isopentyloxyacetic acid [Zhang Jingan: Catalytic Synthesis of Allyl Isoamyloxyacetate. Spices Fragrance Cosmetics, 1995, (4): 31-33]; isopentyloxyacetic acid and allyl alcohol are esterified in the presence of an acid catalyst to obtain Gepongate. Metal sodium requires absolute anhydrous duri...

Claims

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Application Information

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IPC IPC(8): C07C69/708C07C67/08
Inventor 包江峰应登宇徐利红陈绣芳刘训军谢自强
Owner ZHEJIANG XINHUA CHEM
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