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4-nor-amyl diphenic acid-3-fluor-4-cyan phenol ester production process

A technology of n-pentyl bibenzoic acid and pentyl bibenzoic acid is applied in the directions of chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc. The effect of popularizing application prospects, reducing production costs, and reasonable and feasible reaction conditions

Active Publication Date: 2006-11-22
江苏和纯化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] At present, liquid crystal materials have been widely used in electronic and electrical products, but the production process of liquid crystal monomer materials, including the production process of 4-n-pentyl bibenzoic acid-3-fluoro-4-cyanophenol ester liquid crystal monomer materials Haven't seen the report yet

Method used

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  • 4-nor-amyl diphenic acid-3-fluor-4-cyan phenol ester production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1 Production process of 4-n-pentylbibenzoic acid-3-fluoro-4-cyanophenol ester

[0019] (1) Raw materials

[0020] Raw material name Specification index, grade Production unit

[0021] Pentyldibenzoic acid White crystal, melting point ≥ 101.0℃, industrial grade Shijiazhuang Chemical Reagent Co., Ltd.

[0022] Thionyl chloride Yellow-green transparent liquid, industrial grade Changzhou Henglin Chemical Factory

[0023] 3-Fluoro-4-cyanophenol white crystal, melting point≥125℃, industrial grade Shijiazhuang Chemical Reagent Co., Ltd.

[0024] Toluene Colorless transparent liquid, water content ≤0.1%, industrial grade Nanjing Chemical Reagent Co., Ltd.

[0025] Sodium hydroxide White flaky solid, industrial grade; Jiangsu Thorpe Group Co., Ltd.

[0026] Absolute Ethanol Colorless transparent liquid, purity ≥ 99.5%, industrial grade Nanjing Chemical Reagent Co., Ltd.

[0027] (2) Production equipment

[0028] Equipment name Specification model Quantity Manufactu...

Embodiment 2

[0043] Example 2 Production process of 4-n-pentylbibenzoic acid-3-fluoro-4-cyanophenol ester

[0044] The main raw material specifications, production equipment and the molar ratio of the main raw materials pentyl biphenylformic acid, thionyl chloride, 3-fluoro-4-cyanophenol, toluene, sodium hydroxide, and absolute ethanol are the same as in Example 1 ;

[0045] In the production process, when pentyl bibenzoyl chloride and 3-fluoro-4-cyanophenol are esterified and 3-fluoro-4-cyanophenol is added, silica gel and activated carbon are also added at the same time, and the amount of silica gel added is 1kg. Activated carbon addition is 3kg. The quality of the product is improved through the adsorption of impurities in the material by silica gel and the decolorization of the material by activated carbon.

Embodiment 3

[0046] Example 3 Production process of 4-n-pentylbibenzoic acid-3-fluoro-4-cyanophenol ester

[0047] The main raw material specifications, production equipment and the molar ratio of the main raw materials pentyldiphenylformic acid, thionyl chloride, 3-fluoro-4-cyanophenol, toluene, sodium hydroxide, and absolute ethanol are the same as in Example 1 ;

[0048] In the production process, pentyl bibenzoyl chloride and 3-fluoro-4-cyanophenol undergo esterification reaction. When adding 3-fluoro-4-cyanophenol, silica gel and activated carbon are also added at the same time. The amount of silica gel added is 2kg of activated carbon. Addition amount is 4kg. The quality of the product is improved through the adsorption of impurities in the material by silica gel and the decolorization of the material by activated carbon.

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Abstract

This invention relates to a method for producing 4-amyl-biphenylcarboxylic acid-3-fluoro-4-cyanophenol ester, comprising: amyl-biphenylcarboxylic acid, thionyl chloride, 3-fluoro-4-cyanophenol, toluene, sodium-hydroxide, and anhydrous ethyl alcohol as raw material, with mole ration as: amyl-biphenylcarboxylic acid 1.05, thionyl chloride 2.65, 3-fluoro-4-cyanophenol 1, toluene 3, sodium-hydroxide 0.1, and anhydrous ethyl alcohol 4.0. The process comprises two steps: (1) use amyl-biphenylcarboxylic acid and thionyl chloride as raw material for acylation reaction and synthesize amyl-bibenzoyl chloride by normal pressure and decreasing pressure distillation; (2) dropwise add amyl-bibenzoyl chloride and 3-fluoro-4-cyanophenol with toluene as solvent for esterification, and produce the target product 4-amyl-biphenylcarboxylic acid-3-fluoro-4-cyanophenol ester by water washing, alkaline washing, crystallization and recrystallization, wherein the conditions: acylation reaction temperature 160Deg C, reflux time 6h, normal distillation temperature 172-176Deg C, pressure decreasing temperature 118-121Deg C, vacuum 50mmHg, the discharging condition is to collect the 3Deg C range product after temperature and pressure stabilized, the temperature of adding 3-fluoro-4-cyanophenol with agitation for acylation reaction is 100Deg C, keep the temperature between 90 and 100Deg C when dropwise adding amyl-bibenzoyl chloride for 3h, reflux with agitation for 6h, heating steam pressure no more than 0.2MPa, autoclave inside temperature kept at 120+2Deg C, crystallization temperature -15Deg C and kept at -15+-2Deg C for 1h for agitation, recrystallization temperature -15Deg Cand kept at -15+-2Deg C for 1h for agitation.

Description

technical field [0001] The present invention relates to the general method of organic chemistry, particularly a kind of 4-n-pentyl bibenzoic acid-3-fluoro-4-cyanophenol ester production process. Background technique [0002] At present, liquid crystal materials have been widely used in electronic and electrical products, but the production process of liquid crystal monomer materials, including the production process of 4-n-pentyl bibenzoic acid-3-fluoro-4-cyanophenol ester liquid crystal monomer materials Haven't seen reports yet. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for synthesizing pentyl biphenyl with pentyl biphenyl carboxylic acid and thionyl chloride through Friedel-Crafts acylation reaction in view of the lack of reports on the production process of liquid crystal monomers. Formyl chloride, and then the monomer of the target product 4-n...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/55
Inventor 朱康洋
Owner 江苏和纯化学工业有限公司
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