Preparation method of propyldicyclohexyl bromide

A technology of propyl bicyclohexyl and cyclohexyl ketone, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of high processing cost, high risk index, burning effect, etc., to reduce pollution, The effect of improving safety factor and reducing production cost

Inactive Publication Date: 2012-07-25
BENGBU CHINA SYNCHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this preparation method is that the triphenylphosphine added in the reaction will be very difficult to handle, the processing cost is high, and if it is not handled properly, it will cause certain harm to the environment; in addition, the bromine used in the preparation method, its The risk index is high, liquid bromine has a burning effect on the skin, bromine vapor is easy to burn the mucous membrane, and symptoms such as cough, increased mucous membrane secretions, epistaxis, dizziness, etc.

Method used

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  • Preparation method of propyldicyclohexyl bromide
  • Preparation method of propyldicyclohexyl bromide
  • Preparation method of propyldicyclohexyl bromide

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 27.8mol of water and 0.26mol (0.5eq) of sodium borohydride into a 1000ml three-necked reaction flask. After the sodium borohydride is completely dissolved under stirring, slowly add 0.518mol (1.0eq) of propylbicyclohexyl dropwise at room temperature, and then Carry out the reaction at 20°C, and when the reaction system shows more white powder, spot the plate to confirm whether there is any raw material, if there is no, it means that the reaction is complete. After the reaction product was filtered by suction, it was washed with saturated sodium bicarbonate solution, and then washed with water for 3 to 4 times, drained and dried to obtain 0.58 mol of propyl bicyclohexyl alcohol with a water content of 16%, and the yield was greater than 95%. %, for the next bromination reaction. Set up a mechanical stirring device, add 0.067mol (1.0eq) of the above-mentioned propyl bicyclohexyl alcohol into a 250ml three-necked flask, and then add 0.67mol (10eq) of hydrobromic acid t...

Embodiment 2

[0025] Add 8.87mol of ethanol and 0.518mol (1.0eq) of sodium borohydride into a 1000ml three-necked reaction flask. After the sodium borohydride is completely dissolved under stirring, add 0.518mol (1.0eq) of propyl bicyclohexyl ketone dropwise at room temperature, slowly drop Add, let it react at 10°C after the dropwise addition is complete. When the reaction system appears more white powder, spot the board to confirm whether there are raw materials, if there is no, it means that the reaction is complete. After the reaction product was filtered by suction, it was washed with saturated sodium bicarbonate solution, and then washed with clear water for 3 to 4 times, drained and dried to obtain 0.473 mol of propyl bicyclohexyl alcohol with a water content of 20%, and the yield was greater than 92 %. Set up a mechanical stirring device, add 0.067mol (1.0eq) of the above-mentioned propyl bicyclohexyl alcohol into a 250ml three-necked flask, then add 0.335mol (5eq) of HBr into the ...

Embodiment 3

[0027] Add 12.3mol of methanol and 0.78mol (1.5eq) of sodium borohydride into a 1000ml three-necked reaction flask. After the sodium borohydride is completely dissolved under stirring conditions, add 0.518mol (1.0eq) of propylbicyclohexyl dropwise at room temperature, slowly drop Add, because heat will be released during the dropwise addition, after the dropwise addition is complete, let it react at 30°C. When the reaction system appears more white powder, spot the board to confirm whether there are raw materials, if there is no, it means that the reaction is complete. After the reaction product was filtered by suction, it was washed with saturated sodium bicarbonate solution, and then washed 3 to 4 times with clear water, and then dried and air-dried to obtain 0.58 mol of propyl bicyclohexyl alcohol with a water content of 18%, and the yield was greater than 91 %. Set up a mechanical stirring device, add 0.067mol (1.0eq) of the above-mentioned propyl bicyclohexyl alcohol int...

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Abstract

The invention discloses a preparation method of propyldicyclohexyl bromide, which comprises the following steps: reducing propyldicyclohexyl ketone as a raw material with sodium borohydride as a reducing agent to obtain a reduction product of propyldicyclohexyl alcohol, carrying out a bromination reaction of the propyldicyclohexyl alcohol under an action of hydrobromic acid to generate liquid-state propyldicyclohexyl bromide, and carrying out subsequent treatment to obtain solid-state propyldicyclohexyl bromide. Compared with the well-known preparation methods of ethyldicyclohexyl bromide, the preparation method of propyldicyclohexyl bromide disclosed by the invention does not use triphenylphosphine, is simple and convenient in the subsequent treatment, and reduces the degree of environmental pollution. The hazard index of hydrobromic acid used in the preparation method disclosed by the invention is far lower than that of bromine used in the well-known preparation methods of ethyldicyclohexyl bromide so as to increase the safety factor. In addition, hydrobromic acid used in the preparation method disclosed by the invention can be recycled so as to reduce the production cost, and the preparation method lays the foundation for large-scale industrial production of propyldicyclohexyl bromide.

Description

technical field [0001] The invention relates to a liquid crystal display material, in particular to a method for preparing a TFT (thin film transistor) mode liquid crystal display intermediate propyl biscyclohexyl bromide. Background technique [0002] Liquid crystal material is a kind of polymer material. Because of its special physical, chemical and optical properties, it has been widely used in thin and light display technology since the middle of the 20th century. In recent years, liquid crystal materials have developed rapidly along with the development of displays, among which nematic materials for display are the fastest growing type of liquid crystal materials with the largest market share. [0003] Nematic liquid crystal displays include TN (Twisted Nematic) mode, STN (Super Twisted Nematic) mode, and TFT (Thin Film Transistor) mode liquid crystal displays. Among them, propyl bicyclohexyl bromide is an important intermediate of TFT mode liquid crystal display, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C23/18C07C17/16
Inventor 杨青赵士民徐剑霄汪平刘淼刘洪强
Owner BENGBU CHINA SYNCHEM TECH CO LTD
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