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Synthesis method of tert-amylbenzene with controllable isomer content

A technology of tert-amylbenzene and synthetic methods, which is applied in the direction of chemical instruments and methods, hydrocarbons, hydrocarbons, etc., can solve the problems of affecting the yield of products, excessive local reactions, etc., and achieve fast reaction speed and catalyst The effect of small quantity and low price

Pending Publication Date: 2020-06-02
CHINA TIANCHEN ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the reaction process, due to the high activity of aluminum trichloride, the local reaction is too fast; if the generated HCl gas cannot be discharged in time, the tert-amyl group will be rearranged, resulting in a large amount of sec-amylbenzene isomers , thus affecting the yield and further use of the product

Method used

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  • Synthesis method of tert-amylbenzene with controllable isomer content
  • Synthesis method of tert-amylbenzene with controllable isomer content
  • Synthesis method of tert-amylbenzene with controllable isomer content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 220.4g of tert-amyl alcohol into the flask, add 507.6g of concentrated hydrochloric acid (mass concentration: 36.5%) dropwise at 20°C, keep the temperature for 30 minutes after the dropwise addition, and then stop the reaction. The upper organic phase was taken, washed with deionized water, 2% sodium hydroxide solution, and deionized water respectively, and left to stand, and the organic phase was separated. After drying, 261.1 g of tert-amyl chloride product was obtained, with a yield of 98.0%.

Embodiment 2

[0028] Add 220.4g of tert-amyl alcohol into the flask, add 405.7g of hydrobromic acid (mass concentration: 47.0%) dropwise at 50° C., and then keep the temperature for 15 minutes to stop the reaction. The upper organic phase was taken, washed with deionized water, 2% sodium hydroxide solution, and deionized water respectively, and left to stand, and the organic phase was separated. After drying, 364.5 g of tert-amyl bromide was obtained, with a yield of 96.5%.

Embodiment 3

[0030] Add 80.0g of benzene and 1.31g of zinc chloride to the flask, maintain the system at 5°C, vacuumize to an absolute pressure of 50kPa, slowly add 35.1g of tert-amyl chloride and 70.2g of benzene (as a solvent, diluted Tert-amyl chloride) solution, about 1h dropwise to complete. Afterwards, the reaction was continued for 1 h at the temperature and pressure. The reaction solution was poured into 5% dilute hydrochloric acid for hydrolysis, and the organic phase obtained after liquid separation was detected by gas chromatography. It can be seen that the tert-amyl chloride was completely converted, the product yield was 97%, and the ratio of tertiary and secondary isomers was 99.32%. 0.68%.

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Abstract

The invention provides a synthesis method of tert-amylbenzene with controllable isomer content. The synthesis method comprises the following steps: 1) carrying out a substitution reaction on tert-amylalcohol and haloid acid to obtain a halopentane intermediate; 2) carrying out a Friedel-Crafts alkylation reaction on the halopentane intermediate and benzene under the catalysis of a Lewis acid to obtain tert-amylbenzene; wherein the Lewis acid is one of ZnCl2 and FeCl3 or a mixture of the ZnCl2 and the FeCl3; the temperature of the Friedel-Crafts alkylation reaction is -10 to 40 DEG C; the vacuum degree is absolute pressure of 2-75kPa; and the reaction time is 0.5-4 h. According to the synthesis method, by setting reasonable reaction steps, controlling reaction conditions, selecting a proper catalyst and the like, the isomerization ratio is reduced, and the tert-amyl product with high yield and high selectivity is obtained.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and in particular relates to a method for synthesizing tert-amylbenzene with controllable isomer content. Background technique [0002] Tert-amylbenzene (TAB), also known as 2-methyl-2-phenyl-butane, is an important chemical raw material, which can be mainly used in the synthesis of a new hydrogen peroxide working carrier, 2-amylanthraquinone. At present, the main synthesis process of tert-amylbenzene is to make benzene and tert-amyl alcohol as raw materials, with aluminum trichloride as a catalyst, and produce it through Friedel-Crafts alkylation reaction. During the reaction process, due to the high activity of aluminum trichloride, the local reaction is too fast; if the generated HCl gas cannot be discharged in time, the tert-amyl group will be rearranged, resulting in a large amount of sec-amylbenzene isomers , thereby affecting the yield and further use of the product. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/02C07C2/86
CPCC07C2/861C07C17/16C07C2527/128C07C2527/138
Inventor 武金丹陈兴鹏王磊王志明王聪刘新伟杨克俭霍瑜姝
Owner CHINA TIANCHEN ENG
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