1-(2,3,5,6-tetrafluorophenyl)-2,2-dimethylacetone compound and its preparation method

A technology of dimethylacetone and tetrafluorophenyl, which is applied in the field of 1--2,2-dimethylacetonate and its preparation, can solve the problems of high production cost and long synthesis time, and achieve short synthesis time and low cost. Low, the effect of improving the service life

Active Publication Date: 2016-02-24
大连鼎燕医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, liquid crystal materials contain various compounds, which have the disadvantages of long synthesis time and high production cost in the production process. Some compounds have the above-mentioned disadvantages when they are used in medicine and pesticides.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] In a 250ml four-necked round-bottomed flask equipped with a stirrer, a thermometer and a dropping funnel, add 15g of 1,2,4,5-tetrafluorobenzene (0.1mol) and 80ml of tetrahydrofuran, and freeze the mixture with liquid nitrogen acetone It is frozen to -70~-80°C.

[0027] Under vigorous stirring at -70~-80°C, 42ml of n-butyllithium hexane solution (0.105mol) was added dropwise, and the stirring was continued for 30min.

[0028] Under strong stirring at -70~-80°C, add dropwise a solution of 13.6 g of tert-butylformonitrile and 20 ml of tetrahydrofuran, continue stirring for 30 min, and slowly rise to room temperature.

[0029] Transfer the reaction solution to another 500ml round bottom flask at room temperature, add 75ml (1.1mol) of 5% dilute hydrochloric acid with stirring, heat to reflux for 30min, and cool to room temperature.

[0030] Stand at room temperature for stratification, add 20 g of anhydrous magnesium sulfate to the organic phase and stir for 1 h, filter to ...

Embodiment 1

[0031] The processing route of embodiment 1 is

[0032] .

example 2

[0034] In a 250ml four-neck round bottom flask equipped with a stirrer, a thermometer and a dropping funnel, add 16.5g of 2,3,5,6-tetrafluorobenzonitrile (0.1mol), 60ml of tetrahydrofuran, and freeze with liquid nitrogen acetone Freeze it to -70~-80°C.

[0035] Under vigorous stirring at -70~-80°C, 40ml of 16% tert-butyllithium-n-pentane solution (0.102mol) was added dropwise, continued stirring for 30min, and slowly rose to room temperature.

[0036] 75ml (1.1mol) of 5% dilute hydrochloric acid was added dropwise under stirring, heated to reflux for 30min and then cooled to room temperature.

[0037] Stand at room temperature for stratification, add 20g of anhydrous magnesium sulfate to the organic phase and stir for 1 hour, filter to remove inorganic salts, distill off the solvent from the filtrate, stop heating when crystalline solids appear, add 40ml of heptane to cool and crystallize, filter, and dry to obtain white solid crystals 19.2 g. The area percentage of GC is 99...

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PUM

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Abstract

The invention provides a 1-(2, 3, 5, 6-tetrafluorophenyl)-2, 2-dimethyl acetone compound. The structural formula of the 1-(2, 3, 5, 6-tetrafluorophenyl)-2, 2-dimethyl acetone compound is shown in the specification. A synthetic method of the compound comprises the steps that 1, 2, 4, 5-phenyl tetrafluoride serving as a raw material exchanges with n-butyllithium so as to generate 2, 3, 5, 6-tetrafluorophenyl lithium, addition reaction happens between 2, 3, 5, 6-tetrafluorophenyl lithium and tert-butyl formonitrile, and finally the product is obtained through hydrolysis; another synthetic method of the compound comprises the steps that addition reaction happens between 2, 3, 5, 6-phenyl tetrafluoride formonitrile serving as a raw material and tert-butyllithium, and finally the target product is obtained through hydrolysis. The compound provided by the invention has the advantages of short synthetic time and low cost in an application process.

Description

technical field [0001] The invention relates to a novel compound and a preparation method, in particular to a 1-(2,3,5,6-tetrafluorophenyl)-2,2-dimethylacetone compound and a preparation method. Background technique [0002] At present, liquid crystal materials contain various compounds, and the production process has the disadvantages of long synthesis time and high production cost. Some compounds have the above-mentioned disadvantages when they are used in medicine and pesticides. Contents of the invention [0003] The purpose of the present invention is to provide a new compound so as to shorten the synthesis time, reduce the cost and save raw material production in the process of liquid crystal material production, medicine and pesticide production, and overcome the deficiencies of the prior art. [0004] The technical solution of the present invention is: a kind of 1-(2,3,5,6-tetrafluorophenyl)-2,2-dimethylacetone compound, its molecular formula is C 11 h 10 f 4 O,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/807C07C45/42
CPCC07C45/42C07C249/02C07F1/02C07C49/807C07C251/16
Inventor 蔡鲁伯鹿政理范莉莉吕永智董志军吴冬辉李德龙
Owner 大连鼎燕医药化工有限公司
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