Process preparing 2,3,5,6-phyenyl methanol tetrafluoride

A technology of tetrafluorobenzyl alcohol and tetrafluorobenzoyl chloride, applied in 2, can solve problems such as production and use restrictions

Inactive Publication Date: 2007-01-24
常州康美化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 2,3,5,6-Tetrafluorobenzyl alcohol is one of the important intermediates for the synthesis of the pyrethroid pesticide transfluthrin. There have been many reports on its related synth

Method used

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  • Process preparing 2,3,5,6-phyenyl methanol tetrafluoride
  • Process preparing 2,3,5,6-phyenyl methanol tetrafluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0014] In a 500ml four-neck flask, add 0.1mol tetrafluorobenzoyl chloride, directly add 300ml tetrahydrofuran, add 38gNaBH at low temperature 4 , 2g cocatalyst, slowly heat up, control the temperature at 58°C, and react for 8 hours. Cool down and filter with suction. Slowly pour the filtrate into 6% hydrochloric acid solution with stirring to keep the solution acidic. After fully stirring, the organic layer was separated and washed with water to be neutral. The solvent was removed under reduced pressure to obtain 172.7 g of tetrafluorobenzyl alcohol with a purity of 99% and a yield of 95%.

Embodiment 2

[0016] In a 500ml four-neck flask, add 0.1mol tetrafluorobenzoyl chloride, directly add 300ml tetrahydrofuran, add 38gNaBH at low temperature 4 , 10g cocatalyst, and pass into nitrogen protection. Slowly raise the temperature, control the temperature at 86°C, and react for 6 hours. Cool down and filter with suction. Slowly pour the filtrate into 10% hydrochloric acid solution with stirring to keep the solution acidic. After fully stirring, the organic layer was separated and washed with water to be neutral. The solvent was removed under reduced pressure to obtain 176 g of tetrafluorobenzyl alcohol with a purity of 99% and a yield of 96.8%.

Embodiment 3

[0018] In a 500ml four-neck flask, add 0.1mol tetrafluorobenzoyl chloride, directly add 300ml tetrahydrofuran, add 38gNaBH at low temperature 4 , 8g cocatalyst, and pass into nitrogen protection. Slowly raise the temperature, control the temperature at 65°C, and react for 7 hours. Cool down and filter with suction. Slowly pour the filtrate into 8% hydrochloric acid solution with stirring to keep the solution acidic. After fully stirring, the organic layer was separated and washed with water to be neutral. The solvent was removed under reduced pressure to obtain 174.9 g of tetrafluorobenzyl alcohol with a purity of 99% and a yield of 96.2%.

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Abstract

The present invention is process of preparing 2, 3, 5, 6-tetrafluoro phenyl alcohol as one important material for synthesizing tetrafluoro phenyl pyrethrin through the reduction reaction of 2, 3, 5, 6-tetrafluoro benzoyl chloride material under the action of solvent, reductant and assistant.

Description

technical field [0001] The invention relates to a new preparation method of 2,3,5,6-tetrafluorobenzyl alcohol (abbreviation: tetrafluorobenzyl alcohol), an important intermediate for synthesizing transfluthrin. Background technique [0002] 2,3,5,6-Tetrafluorobenzyl alcohol is one of the important intermediates for the synthesis of the pyrethroid pesticide transfluthrin. There have been many reports on its related synthesis methods at home and abroad, and many of them have applied for patent protection , such as DE2658074, GB2155464, CN1349484A, etc., make the production and use of this product restricted. The present invention emphatically introduces a new synthetic method that is simple and efficient, high-quality and high-yield industrial production, and obtains 2 by reduction of 2,3,5,6-tetrafluorobenzoyl chloride (abbreviation: tetrafluorobenzoyl chloride). , 3,5,6-tetrafluorobenzyl alcohol, so as to further synthesize transfluthrin. Contents of the invention [000...

Claims

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Application Information

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IPC IPC(8): C07C29/147C07C33/46
Inventor 陈建海吴小燕
Owner 常州康美化工有限公司
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