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A method for preparing s-(+)-4-(2-methylbutyl) biphenol

A technology of methylbutyl and biphenol is applied in the field of preparing liquid crystal intermediate materials and preparing S-(+)-4-(2-methylbutyl)biphenol, which can solve harsh operating conditions and process reaction steps. Cumbersome, difficult to achieve industrialized preparation and other problems, to achieve the effect of easy mass production, simple process and low cost

Active Publication Date: 2017-07-18
HEBEI YANUO CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although (S)-(+)-4-(2-methylbutyl)biphenol has the above-mentioned better uses, after searching, the existing literature has no The preparation method of S-(+)-4-(2-methylbutyl)biphenol has been reported less, and the preparation method of S-(+)-4-(2-methylbutyl)biphenol is as follows: Shunji Uchida et al. 2-Methylbutyric acid is used as raw material, reacts with thionyl chloride to generate (S)-2-methylbutyryl chloride, and butyryl chloride reacts with 4-methoxybiphenyl to obtain 4-methoxy- 4-(2-methylbutyryl)biphenyl, the intermediate is reduced with zinc powder to give 4-methoxy-4-(2-methylbutyl)biphenyl, which is reacted with boron tribromide at -70°C Demethylation reaction occurs to obtain S-(+)-4-(2-methylbutyl) biphenol. The reaction steps of this process are cumbersome and the operating conditions are harsh, so it is difficult to realize industrial production

Method used

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  • A method for preparing s-(+)-4-(2-methylbutyl) biphenol
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  • A method for preparing s-(+)-4-(2-methylbutyl) biphenol

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Embodiment 1

[0038] The preparation of embodiment 1 S-(+)-4-(2-methylbutyl) biphenyl ethyl ketone

[0039] Install a mechanical stirrer and a thermometer in a dry 1-liter four-necked bottle. Add 250mL of dichloromethane and 75g of aluminum trichloride to the four-neck bottle, and lower the temperature to T99%, and the total yield>85%.

Embodiment 2

[0040] Example 2 Preparation of S-(+)-4-(2-methylbutyl)biphenol

[0041] Take a 2-liter four-necked bottle and install a mechanical stirrer and a thermometer. Add 27g of S-(+)-4-(2-methylbutyl)biphenylphenone, 500mL of acetic acid, 100g of concentrated sulfuric acid, and 100g of water into the four-neck flask, and when the temperature rises to T=50°C, add 60g of potassium persulfate, Insulated and stirred for 4.5 hours. After the reaction, 500 mL of water was added to the reaction solution, stirred for 10 minutes, solids were precipitated, filtered with suction, the filter cake was washed with water and neutralized, and 23 g of the product was obtained after the filter cake was dried. Add 60 mL of Toluene, heat to dissolve, heat filter, add 30mL of petroleum ether to the filtrate, put it in a refrigerator at -10°C after dissolving, overnight, recrystallize and filter to obtain a needle-shaped solid, weigh it, and then continue to add three times of toluene, 1.5 times of petro...

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Abstract

The invention discloses a method for preparing S-(+)-4-(2-methylbutyl) biphenol. S-(+)-4-(2-methylbutyl)biphenyl, acetyl chloride and aluminum trichloride are used as raw materials to prepare S-(+)-4-(2-methylbutyl)biphenyl ketone; then the obtained S-(+)-4-(2-methylbutyl) benzophenone is reacted with oxidant potassium persulfate to obtain S-(+)-4-(2-methylbutyl) phenol. The invention prepares S-(+)-4-(2-methylbutyl) biphenol through two-step reaction, has a simple process and is suitable for batch production. The biphenol prepared by the invention is used in the synthesis of liquid crystal materials for TFT displays, and is used as an inducer in mixed liquid crystal formulations to obtain products with high stability and low phase transition temperature, and has wide application prospects.

Description

technical field [0001] The invention relates to a method for preparing liquid crystal intermediate materials, in particular to a method for preparing S-(+)-4-(2-methylbutyl)biphenol, which belongs to the technical field of organic chemical industry. Background technique [0002] Chiral additives are important components of liquid crystal materials for display. As early as the 20th century, Friedel discovered that adding a small amount of optically active substances to nematic liquid crystals can induce the transformation of nematic phase into cholesteric phase. Fifty years later, Bulkingham and Stegemeyer conducted systematic research on this phenomenon. The earliest chiral additives used were ester derivatives of cholesterol until Gray synthesized (+)-(2-methylbutyl)-4-cyanobiphenyl (code name BC-15) in the mid-1970s. After that, chiral additives developed rapidly. The twisting force (HTP) is an important parameter to evaluate the twisting ability of chiral additives, ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/15C07C37/50
CPCC07C37/50C07C45/46C07C39/15C07C49/784
Inventor 刘晓民刘俊娟温宁史洪波张明翠李新明李书建凌广轩梁建国李永辉相聪张伟燕赵丽雅吴浪王佳柳张漫李学燕王盼芹李燕川聂文娜
Owner HEBEI YANUO CHEM IND