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Preparation method of 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol

A xylyl and o-xylene technology, which is applied in the field of preparation of 2--1,1,1,3,3,3-hexafluoro-2-propanol, can solve the problems of potential safety hazards and high reaction pressure

Inactive Publication Date: 2017-05-24
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method described in this patent needs to use hexafluoropropylene oxide gas, the reaction pressure is high, and there are potential safety hazards

Method used

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  • Preparation method of 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol

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Experimental program
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Effect test

Embodiment 1

[0021] In a 500mL three-necked flask equipped with a water separator, add 110g (0.5mol) of hexafluoroacetone trihydrate and 212g (2mol) of o-xylene, separate layers, stir, and the reaction liquid is a milky white mixture, which is heated to reflux temperature, about At 94°C, water separates from the water separator (approximately 45g o-xylene is added to the water separator), and continues to heat and reflux until almost no water is released. The liquid in the reaction bottle is colorless and transparent, which is a mixture of o-xylene and hexafluoroacetone. Hydrate mixture; transfer the above-mentioned mixture of o-xylene and hexafluoroacetone monohydrate to a 1L vacuumed autoclave, add 60g of anhydrous hydrogen fluoride, raise the temperature to 85°C, and react for about 13 hours at a reaction pressure of about 4.2atm. After the reaction, lower the temperature, release the pressure, blow with nitrogen three times, wash and absorb the tail gas with water and alkali, open the k...

Embodiment 2

[0023] In a 500mL three-necked flask equipped with a water separator, add 110g (0.5mol) of hexafluoroacetone trihydrate and 106g (1mol) of o-xylene, separate layers, stir, the reaction solution is a milky white mixture, heat up to reflux temperature, and separate Water was separated from the water tank (approximately 45 g of o-xylene was added to the water separator), and the heating and reflux was continued until almost no water was released. The liquid in the reaction bottle was colorless and transparent, and was a mixture of o-xylene and hexafluoroacetone monohydrate; Transfer the above-mentioned mixture of o-xylene and hexafluoroacetone monohydrate to a 1L vacuumed autoclave, add 55g of anhydrous hydrogen fluoride, raise the temperature to 100°C, and react for about 17 hours at a reaction pressure of about 3.7 atm. After the reaction, Lower the temperature, release the pressure, purging three times with nitrogen, wash and absorb the tail gas with water and alkali, open the ...

Embodiment 3

[0025] In a 250mL three-necked flask equipped with a water separator, add 75g (0.34mol) of hexafluoroacetone trihydrate and 61g (0.58mol) of o-xylene, separate layers, stir, the reaction solution is a milky white mixture, and the temperature is raised to reflux temperature, There is water separated in the water separator (approximately 45g o-xylene is added to the water separator), continue to heat and reflux until almost no water is released, the liquid in the reaction bottle is colorless and transparent, which is a mixture of o-xylene and hexafluoroacetone monohydrate ;Transfer the mixture of o-xylene and hexafluoroacetone monohydrate above to a 1L vacuumed autoclave, add 22g of anhydrous hydrogen fluoride, heat up to 70°C, react for about 10h, and the reaction pressure is about 2.3atm. , lower the temperature, remove the pressure, purged three times with nitrogen, wash and absorb the tail gas with water and alkali, open the kettle, pour the reaction solution into ice water w...

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Abstract

The invention provides a method for preparing 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol. The 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol is prepared from o-xylene and hexafluoroacetone monohydrate under the action of hydrogen fluoride via a liquid-phase reaction. The method provided by the invention is low in raw material toxicity, low in reaction pressure, easy to operate, high in reaction selectivity and yield and suitable for industrial production. The prepared 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol is suitable for being used as a fluorine-containing medical intermediate.

Description

technical field [0001] The invention relates to a preparation method of 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol. Background technique [0002] 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol is an important fluorine-containing pharmaceutical intermediate, with the following structural formula (I): [0003] [0004] For the preparation method of 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol, there are following reports in the prior art: [0005] Japanese patent JP2006248963 discloses a preparation method of 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol, using hexafluoroacetone as raw material, hydrogen fluoride As a catalyst, the organic layer obtained after the reaction was analyzed by gas chromatography to obtain 2-(3,4-xylyl)-1,1,1,3,3,3-hexafluoro-2-propanol and 2,2- The peak area ratio of bis(3,4-xylyl)hexafluoropropane was 91.2:8.8. This patent has no reaction yield report. The method described in this patent requires the use of highly toxic and expen...

Claims

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Application Information

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IPC IPC(8): C07C29/38C07C33/46
CPCC07C29/38C07C33/46
Inventor 赵卫娟徐卫国杨箭张勇耀
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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