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Preparation method of 1-chlorin-4-ethoxy-2,3-difluorobenzene

A technology of ethoxy and difluorobenzene, applied in the field of 1-chloro-4-ethoxy-2

Inactive Publication Date: 2012-07-04
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the preparation of this compound, there is no report in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] In a 250ml three-necked flask, add 120ml of chloroform, 50g of 2,3-difluorophenetole, 0.3g of reduced iron powder, start stirring, and lower the temperature. When the temperature drops to -2 degrees Celsius, through the constant pressure dropping funnel Charge 52.3g of chlorine, complete the charge in about 1 hour, keep the reaction temperature at -2 to -8 degrees Celsius, react for 3 hours, and stop the reaction. Add 50ml of aqueous solution (15g of sodium bisulfate dissolved in 50ml of water) to the reaction solution, stir for 0.5h, separate the layers, and wash the lower organic phase with water for 3 to 5 times until neutral. The organic phase was dried with 20 ml of anhydrous sodium sulfate for 2 h, concentrated, and sampled and analyzed to obtain about 75 g of a crude product with a content of 97.1%. Pour 75g of the crude product into a 250ml beaker, recrystallize with petroleum ether, stir, and cool to -2 to -5 degrees Celsius to slowly precipitate crystals. Put...

Embodiment 2

[0012] In a 250ml three-necked flask, add 220ml of chloroform, 80g of 2,3-difluorophenetole, 0.4g of reduced iron powder, start stirring, and lower the temperature. When the temperature drops to -2 degrees Celsius, through the constant pressure dropping funnel Charge 72.3g of chlorine, complete the charge in about 1 hour, keep the reaction temperature at -2 to -5 degrees Celsius, react for 3 hours, and stop the reaction. Add 50ml of aqueous solution (15g of sodium bisulfate dissolved in 50ml of water) to the reaction solution, stir for 0.5h, separate the layers, and wash the lower organic phase with water for 3 to 5 times until neutral. The organic phase was dried with 30 ml of anhydrous sodium sulfate for 2 h, concentrated, and sampled and analyzed to obtain about 97 g of a crude product with a content of 97.1%. Pour 97g of the crude product into a 250ml beaker, recrystallize with petroleum ether, stir, and cool to -2 to -5 degrees Celsius to slowly precipitate crystals. Put...

Embodiment 3

[0014] In a 250ml three-necked flask, add 150ml of chloroform, 60g of 2,3-difluorophenetole, 0.39g of reduced iron powder, start stirring, and lower the temperature. When the temperature drops to -2 degrees Celsius, the Charge 44.9g of chlorine, complete the charge in about 1 hour, keep the reaction temperature at -2 to -8 degrees Celsius, react for 3 hours, and stop the reaction. Add 50ml of aqueous solution (15g of sodium bisulfate dissolved in 50ml of water) to the reaction solution, stir for 0.5h, separate the layers, and wash the lower organic phase with water for 3 to 5 times until neutral. The organic phase was dried with 20 ml of anhydrous sodium sulfate for 2 h, concentrated, and sampled and analyzed to obtain about 69 g of a crude product with a content of 95.1%. Pour 69g of the crude product into a 250ml beaker, recrystallize with petroleum ether, stir, and cool to -2 to -5 degrees Celsius to slowly precipitate crystals. Put it in the refrigerator for 4 hours, and ...

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PUM

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Abstract

The invention provides a preparation method of 1-chlorin-4-ethoxy-2,3-difluorobenzene. The 1-chlorin-4-ethoxy-2,3-difluorobenzene is synthesized by taking 2,3-difluorobenzene ether and chorine as raw materials and taking reduced iron powder as a catalyst. Reaction operation is simple and practicable, and the method has industrial production application value.

Description

technical field [0001] The invention relates to the field of fluorine chemical industry, in particular to a synthesis method of 1-chloro-4-ethoxy-2,3-difluorobenzene. Background technique [0002] With the rapid development of the information industry, liquid crystals have been used in various fields, especially in the field of flat panel display, where liquid crystals have been widely used. According to different functions and needs, the requirements for liquid crystal display technology and liquid crystal materials are also constantly increasing. 1-Chloro-4-ethoxy-2,3-difluorobenzene is an important raw material for the synthesis of liquid crystal intermediates, which is expensive and made from 1-chloro-4-ethoxy-2,3-difluorobenzene Compared with the existing liquid crystal materials, the performance of the liquid crystal material has been greatly improved. Due to the introduction of lateral double fluorine atoms, it has a large negative dielectric anisotropy, a very wide ...

Claims

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Application Information

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IPC IPC(8): C07C43/225C07C41/22
Inventor 张巍谢西平柳叶
Owner SHANGHAI SINOFLUORO SCI
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