Method for synthesizing metoxyl acetophenone

A technology of methoxyacetophenone and synthesis method, which is applied in the field of chemical synthesis, can solve the problems such as complicated preparation process of Hβ zeolite molecular sieve, unsuitability for large-scale production, and difficult control of adsorption balance, so as to achieve no ecological environment risk and improve product quality. Yield and purity, low cost effect

Active Publication Date: 2013-09-18
SHENZHEN UV-CHEMTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of the Hβ zeolite molecular sieve used in this method is complicated, the regeneration temperature is high, the adsorption balance is difficult to control, the catalytic reaction is selective, the experimental cost is high, and it is not suitable for large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Control the internal temperature at 10-15°C, and slowly add 108g of anisole, 10.2g of acetic anhydride and 204g of zinc chloride to a 500mL three-necked flask in sequence, mix and stir for 2 hours, then slowly add 114g of acetic anhydride dropwise again, After 2 hours of dripping, after the solution turns from colorless-pink-red-purple in turn, keep warm for 20min; then raise the temperature to 25°C and keep warm for 1h;

[0025] (2) Add dichloromethane to step (1), heat up to 35° C., cool to room temperature after reacting for 2 hours, add 10% sodium hydroxide solution to adjust pH to 5-6, let stand, and separate layers;

[0026] (3) In the step (2), the upper organic phase is distilled under normal pressure to separate dichloromethane; through vacuum distillation, at 31mmHg, the internal temperature is controlled to 68-78°C, and the mixture of acetic anhydride and glacial acetic acid is separated; continue to heat up to 163~164°C, a colorless product of p-...

Embodiment 2

[0030] (1) Control the internal temperature at 10~15°C, and slowly add 86g of anisole, 5.2g of acetic anhydride and 163g of zinc chloride into a 500mL three-necked bottle in turn, mix and stir for 1.5 hours, then slowly add 91g of acetic anhydride dropwise, 1.5 After dropping for 2 hours, after the solution turns from colorless-pink-red-purple in turn, keep warm for 30min; then raise the temperature to 25°C and keep warm for 1h.

[0031] (2) Add dichloromethane to step (1), heat up to 35°C, react for 2 hours, cool to room temperature, add 10% sodium hydroxide solution to adjust pH to 5-6, let stand, and separate layers.

[0032] (3) In step (2), the upper organic phase is distilled under normal pressure to separate dichloromethane; through distillation under reduced pressure, at 31mmHg, the internal temperature is controlled to 40 ~ 50°C, and the mixture of acetic anhydride and glacial acetic acid is separated; continue to heat up to 163~164°C, a colorless product of p-methoxy...

Embodiment 3

[0036] (1) Control the internal temperature at 10-15°C, slowly add 129g of anisole, 12.5g of acetic anhydride and 245g of zinc chloride into a 500mL three-necked bottle in turn, mix and stir evenly, slowly add 145.5g of acetic anhydride dropwise for 2 hours After dripping, wait for the solution to turn from colorless-pink-red-purple in turn, keep warm for 20min; then raise the temperature to 25°C, keep warm for 1h.

[0037] (2) Add dichloromethane to step (1), heat up to 35°C, react for 2 hours, cool to room temperature, add 10% sodium hydroxide solution to adjust pH to 5-6, let stand, and separate layers.

[0038] (3) The upper organic phase in the step (2) is distilled under normal pressure to separate dichloromethane; through distillation under reduced pressure, at 31mmHg, the internal temperature is controlled to 85 ~ 100°C, and the separation obtains the mixture of acetic anhydride and glacial acetic acid; continue to heat up to 163~164°C, a colorless product of p-methoxy...

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Abstract

The invention relates to a method for synthesizing metoxyl acetophenone. The high-yield and high-purity metoxyl acetophenone is synthesized from anisole and acetic anhydride in the presence of zinc chloride serving as a catalyst and dichloromethane serving as a solvent through Friedel-Crafts acylation reaction under normal temperature condition. The method is simple in synthesis process, low in cost and gentle in reaction condition, the synthesis yield is improved to 90%, the purity is 99.5%, and meanwhile waste liquid is well used to prepare the zinc chloride. The method is free of environmental risk, remarkable in economic benefits and applicable to large-scale production.

Description

technical field [0001] The invention relates to a synthesis method of p-methoxyacetophenone, specifically a green synthesis method for synthesizing p-methoxyacetophenone through Friedel-Crafts acylation reaction using anisole and acetic anhydride as raw materials, which belongs to chemical synthesis field. Background technique [0002] P-methoxyacetophenone is an important spice, medicine, and cosmetic intermediate. Anisole is prepared by Friedel-Crafts acylation reaction to p-methoxyacetophenone, which is an important class of fine chemical and pharmaceutical industries. reaction. At present, p-methoxyacetophenone is still in the research and development stage in China, and the traditional process often uses Lewis acid (ZnCl 2 ) The catalyst is synthesized in a homogeneous phase, the catalyst is often 2 to 3 times in excess, and the reflux temperature is as high as 140°C. The catalytic activity is extremely low, and only a small amount of products can be converted. Sever...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/46C01G9/02
Inventor 李德江陈义星王艳玲李永双
Owner SHENZHEN UV-CHEMTECH CO LTD
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