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Preparation method of Etocrilene

A technology based on Lilin and the preparation process, applied in the preparation of organic compounds, carboxylic acid nitrile preparation, chemical instruments and methods, etc., can solve the problems of reduced reaction yield and achieve improved conversion rate, less impurities and high purity Effect

Inactive Publication Date: 2019-08-23
武汉本杰明医药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Application No. 201811381161.4 discloses a preparation process of Lilin, which takes away the water generated in the reaction process through vacuum distillation. While taking away the water, it will also take away the acetic acid, resulting in a decrease in the reaction yield.

Method used

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  • Preparation method of Etocrilene
  • Preparation method of Etocrilene
  • Preparation method of Etocrilene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 (adding acetic acid midway)

[0031] Put 580kg of benzophenone, 520kg of ethyl cyanoacetate, 70kg of ammonium acetate and 60kg of acetic acid into the synthesis kettle in proportion, raise the temperature to 45°C, stir and dissolve; put on a vacuum, and gradually evacuate until there is an appropriate amount of distillate in the condenser (about -0.088Mpa), start to calculate the reaction time, continue to heat up to 72°C, keep warm, and gradually increase the vacuum until it reaches -0.095Mpa;

[0032] Add 50kg of preset amount of acetic acid to the reaction vessel, cancel the vacuum, and the reaction time is 10h;

[0033] After the reaction is over, turn on the circulating water to cool down to below 60°C under the condition of vacuum, add 300kg of water, stir for 20 minutes, stop the stirring, and keep it for 30 minutes. This process will cause stratification; extract the lower oil layer (the upper layer of waste water layer is discharged into the waste...

Embodiment 2

[0034] Embodiment 2 (adding acetic anhydride midway)

[0035] Put 580kg of benzophenone, 520kg of ethyl cyanoacetate, 70kg of ammonium acetate and 60kg of acetic acid into the synthesis kettle in proportion, raise the temperature to 45°C, stir and dissolve; put on a vacuum, and gradually evacuate until there is an appropriate amount of distillate in the condenser (about -0.088Mpa), start to calculate the reaction time, continue to heat up to 72°C, keep warm, and gradually increase the vacuum until it reaches -0.095Mpa;

[0036] Add 50kg of preset amount of acetic acid to the reaction vessel, cancel the vacuum, and the reaction time is 10h;

[0037] After the reaction is over, turn on the circulating water to cool down to below 60°C under the condition of vacuum, add 300kg of water, stir for 20 minutes, stop the stirring, and keep it for 30 minutes. This process will cause stratification; extract the lower oil layer (the upper layer of waste water layer is discharged into the ...

Embodiment 3

[0038] Embodiment 3 (addition of acetic anhydride+catalyst 1,3-dialkylimidazole oxometalate midway)

[0039] Put 580kg of benzophenone, 520kg of ethyl cyanoacetate, 70kg of ammonium acetate, 60kg of acetic acid, and 6.1kg of 1,3-dialkylimidazolium oxometalate into the synthesis kettle in proportion, raise the temperature to 45°C, and stir to dissolve; Apply vacuum and gradually evacuate until there is an appropriate amount of distillate in the condenser (about -0.088Mpa), start to calculate the reaction time, continue to heat up to 72°C, keep warm, and gradually increase the vacuum until it reaches -0.095Mpa;

[0040] Add 50kg of preset amount of acetic acid to the reaction vessel, cancel the vacuum, and the reaction time is 10h;

[0041] After the reaction is over, turn on the circulating water to cool down to below 60°C under the condition of vacuum, add 300kg of water, stir for 20 minutes, stop the stirring, and keep it for 30 minutes. This process will cause stratification...

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Abstract

The invention discloses a preparation method of Etocrilene. The method comprises the following steps: 1), benzophenone, ethyl cyanoacetate, ammonium acetate and acetic acid are added into a reaction container in proportion, and then are heated and dissolved; 2), vacuumizing is performed gradually to reach a preset vacuum degree, the temperature is raised to a first preset temperature, and then iskept, a preset amount of acetic anhydride is added into the reaction container, and a reaction is carried out for 8-12 h; and 3), the container is cooled to a second preset temperature, the obtained reaction product is washed with water, stands and stratifies, and the obtained upper oil layer is taken, cooled for crystallization, filtered and dried to obtain the target product Etocrilene. The prepared Etocrilene has a high purity and few impurities; and the acetic anhydride is added in the preparation process, and a two-catalyst mode combining 1,3-dialkylimidazolium oxometallate and acetic acid is adopted to replace a traditional single-catalyst mode, so the conversion rate is greatly improved.

Description

technical field [0001] The present invention relates to the field of etocrine preparation. More specifically, the present invention relates to a preparation process of ertoridine. Background technique [0002] UV absorber etocrine, chemical name: ethyl 2-cyano-3,3-diphenylacrylate, chemical structure: Appearance: white crystalline powder, English name: Etocrilene, abbreviated as ETO; used in plastics, paints, dyes, automotive glass, cosmetics, sunscreens as UV absorbers, and it is also a synthetic UV absorber octocrylene an important intermediate. [0003] Application No. 201811381161.4 discloses a preparation process of Lilin, in which the water produced in the reaction process is taken away by vacuum distillation. While taking away the water, it will also take away the acetic acid, resulting in a decrease in the reaction yield. Contents of the invention [0004] In order to achieve the above object, the present invention provides a preparation process of ertocrine, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/41
CPCC07C253/30C07C255/41
Inventor 胡林林
Owner 武汉本杰明医药股份有限公司
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