Preparation technology of styrallyl acetate

A technology of styroyl acetate and preparation process, which is applied in the preparation of carboxylate, the preparation of organic compounds, organic chemistry, etc., can solve the problems of difficult mass production, dangerous reaction process, and high raw material prices, and achieves high synthetic product content, The effect of low reaction temperature and high selectivity

Active Publication Date: 2012-04-25
黄山科宏生物香料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The steps of the above several methods for synthesizing styroyl acetate are relatively complicated, and two-step chemical reactions are required to synthesize the product
The first method is dangerous to feed chlorine and the reaction process is difficult to control; the second method has relatively high raw material prices and is not easy for large-scale production; the third method needs to be replaced by nitrogen and hydrogen during the reaction process, which is not easy to control, and with the With the continuous improvement of the price of acetophenone, it is necessary to develop a new process that is more green, environmentally friendly and cheap

Method used

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  • Preparation technology of styrallyl acetate
  • Preparation technology of styrallyl acetate
  • Preparation technology of styrallyl acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0030] In a 500ml round-bottomed flask equipped with a thermometer, stirrer and reflux condensing device, add 3g of lanthanum bromide, 100g of styrene and 90g of acetic acid in sequence, heat up while stirring, and control the temperature at 120°C. After 15 hours of reaction , unreacted acetic acid and styrene in the reaction solution were recovered by distillation under reduced pressure, and then the fraction at 94-96° C. / 12 mmHg was collected by vacuum distillation to obtain 55 g of styringyl acetate product with a content of 97.5%. Gas chromatography analysis showed that the conversion rate of styrene reached 48%, and the selectivity was 87%.

Embodiment 2

[0032] In a 500ml round bottom flask equipped with a thermometer, stirrer and reflux condensing device, add 5g of lanthanum bromide, 100g of styrene and 120g of acetic acid in sequence, and heat up while stirring, controlling the temperature at 105°C. After 8 hours of reaction , unreacted acetic acid and styrene in the reaction solution were recovered by distillation under reduced pressure, and then the fraction at 94-96° C. / 12 mmHg was collected by vacuum distillation to obtain 59 g of styringyl acetate product with a content of 98%. Gas chromatography analysis showed that the conversion rate of styrene reached 50%, and the selectivity was 90%.

Embodiment 3

[0034] In a 500ml round-bottomed flask equipped with a thermometer, stirrer and reflux condensing device, add 4g of lanthanum chloride, 100g of styrene and 80g of acetic acid in sequence, heat up while stirring, and control the temperature at 110°C. After 12 hours of reaction , unreacted acetic acid and styrene in the reaction solution were recovered by distillation under reduced pressure, and then the fraction at 94-96° C. / 12 mmHg was collected by vacuum distillation to obtain 50.7 g of styringyl acetate product with a content of 97%. Gas chromatography analysis showed that the conversion rate of styrene reached 50%, and the selectivity was 78%.

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Abstract

The invention relates to a preparation technology of styrallyl acetate. Raw materials of styrene and acetate in a mass ratio of 1:0.5-1.5 are treated with a one-step addition reaction under catalysis of rare earth halogenate salt to generate styrallyl acetate with a content higher than 97%. The invention has high selectivity and a simple technology, which only requires the one-step reaction to synthesize the styrallyl acetate; the used raw materials of styrene and acetate are easily available and cheap; used equipment is simple and conveniently operated; and the technology has good selectivity, little by-product and little pollution, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation process of styroyl acetate. Background technique [0002] Perfume is a substance that can be smelled or tasted. It is the raw material for preparing essence. Among many spices, carboxylic acid esters are very important spices with a wide range of uses and a large amount. Among them, styroyl acetate It is a kind of natural equivalent spices and artificial spices. It has a sweet and powerful leaf green smell, which is also like the fragrance of gardenia, and has a hot and sour, green berry fragrance. It is mainly used as a deodorant for gardenia, evening Fragrant jade, hyacinth, lilac, jasmine, lily of the valley and other daily flavors; and it is one of the food flavors allowed by the state, used in apple, pineapple, peach, apricot and other food flavors. The chemical name of styroyl acetate is α-methylbenzyl acetate, and its molecular structure is: [0...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07C69/157C07C67/04
Inventor程存照
Owner黄山科宏生物香料股份有限公司