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Method for preparing 2,6-difluorobenzonitrile by using 2,6-dichlorobenzonitrile fluoro

A technology of dichlorobenzonitrile and difluorobenzonitrile, applied in 2, can solve the problems of cumbersome reaction operation, long reaction cycle, and large amount of solvent used, and achieve good technical effect, easy operation, and less solvent amount

Inactive Publication Date: 2003-09-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to overcome the problems in the previous literature that only high-content 2,6-DCBN can be used as raw materials, the amount of solvent used in the reaction process is large, the reaction operation is cumbersome, and the reaction cycle is long. Problems, to provide a new The method for preparing 2,6-difluorobenzonitrile by fluorination of 2,6-dichlorobenzonitrile

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0017] Add 27.3 grams of dichlorobenzonitrile crude product (mass fraction is 75.1%), 50.0 grams of toluene in the 250 milliliter three-necked flask that has agitator, condenser, thermometer, heat to reflux, change to normal temperature when there is no obvious water droplet. Toluene was removed by pressure distillation (the measured water content was 4.4 g), and then 2,6-dichlorotoluene was distilled off at 130° C. / 13 kPa (this is the starting material for the preparation of 2,6-dichlorobenzonitrile). Cooling, add sulfolane 70.0 milliliters, anhydrous potassium fluoride 17.4 grams (0.30 mole) and C m h 2m+1 O(C n h 2n+1 O) x C m h 2m+1 (n=2, m=1, average molecular weight M: 600) 0.5 g, heated up to 250° C. under rapid stirring, and kept at this temperature for 3.5 hours. After the reaction, 12.7 grams of the product at 92-98° C. / 2.5 kPa were collected by vacuum rectification, the yield of 2,6-DFBN was 91.5%, and the mass fraction was 99.2%. Sulfolane was recovered and ...

Embodiment 3

[0018] Add 21.3 grams of dichlorobenzonitrile crude product (mass fraction is 96.0%), 50.0 grams of toluene in the 250 milliliter three-necked flask that has agitator, condenser, thermometer, heat to reflux, change to normal temperature when there is no obvious water drop. Toluene was removed by pressure distillation (3.4 grams of water was measured), and then 2,6-dichlorotoluene was distilled off at 130°C / 13kPa (this is the starting material for the preparation of 2,6-dichlorobenzonitrile). Cool, add sulfolane 85.7 milliliters, anhydrous potassium fluoride 29.0 grams (0.50 mole) and C m h 2m+1 O(C n h 2n+1 O) x C m h 2m+1 (n=3, m=2, average molecular weight M: 1200) 1.2 g, heated up to 230° C. under rapid stirring, and kept at this temperature for 5.0 hours. After the reaction, vacuum rectification collected 12.2 grams of product at 92-98°C / 2.5kPa, the yield of 2,6-DFBN was 87.7%, and the mass fraction was 99.1%. Sulfolane was recovered and used mechanically after furt...

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Abstract

The present invention adopts 2,6-dichlorobenzonitrile crude product as raw material, uses sulfolane as solvent and uses low-grade polyaliphatic alcohol ether compound as catalyst, under the conditions of that its reaction temp. is 170-250 deg.C and reaction pressure is normal pressure make the above-mentioned materials produce reaction for 2-5 hr, so as to obtain the invented product 2,6-difluorobenzonitrile.

Description

technical field [0001] The invention relates to a method for preparing 2,6-difluorobenzonitrile by fluorinating 2,6-dichlorobenzonitrile. Background technique [0002] 2,6-Difluorobenzonitrile (2,6-Difluorobenzonitrile, 2,6-DFBN for short) is an important intermediate for the synthesis of benzoylurea insecticides. Benzoylurea compounds have a unique insecticidal mechanism, are highly selective, use less, and are environmentally friendly. They are known as green pesticides in the 21st century and are valued by pesticide synthesis and plant workers. The development of this The production technology of quasi-intermediates is becoming more and more important. [0003] The method of the synthetic fluorobenzonitrile of domestic and foreign reports mainly contains following several: (1) take 2,6-dichlorobenzonitrile (2,6-DCBN) as raw material fluorination synthetic 2,6-DFBN; ( 2) Using 2,3,6-trichlorobenzonitrile as a raw material to synthesize DFBN...

Claims

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Application Information

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IPC IPC(8): C07C253/14C07C253/30C07C255/50
Inventor 陈金华沈之芹金文清胡永君杨霞琴
Owner CHINA PETROLEUM & CHEM CORP
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