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A kind of preparation method of chloromethyl hexafluoroisopropyl ether

A technology of chloromethyl hexafluoroisopropyl ether and hexafluoroisopropyl alcohol, which is applied in the field of preparation of chloromethyl hexafluoroisopropyl ether, can solve the problem that it is not suitable for industrial production, cannot meet industrial production, and the final product contains a large amount of impurities and other problems, to achieve the effect of solving the curing phenomenon, reducing the difficulty of purification, and reducing the content of acetal impurities

Active Publication Date: 2021-11-16
JIANGSU HENGRUI MEDICINE CO LTD +2
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Therefore, strong acid is easy to react with polyethylene glycol to generate impurities during the heating process, and it will also react with metal fluoride to generate highly toxic hydrogen fluoride, and it will also react with the product sevoflurane to cause sevoflurane to degrade, making the final product contain a large amount of impurities. Suitable for industrial production
[0007] Although the preparation methods of multiple chloromethyl hexafluoroisopropyl ethers are disclosed in the prior art, most of them have deficiencies and cannot meet the requirements of industrial production

Method used

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  • A kind of preparation method of chloromethyl hexafluoroisopropyl ether

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Effect test

Embodiment 1

[0024] Add 310kg of aluminum trichloride and 210kg of chloromethyl hexafluoroisopropyl ether into a 1000L reactor, cool down to -5°C to 0°C, add 300kg of hexafluoroisopropanol dropwise under stirring, and continue stirring for 0.5 Hour, add 56.8kg paraformaldehyde again, reaction temperature is lower than 35 ℃, continue to react for 17 hours. Lower the temperature below 0°C, add 600L of 6mol / L hydrochloric acid dropwise, and the temperature during the dropwise addition of hydrochloric acid should not exceed 15°C. The organic layer was separated and washed twice with 600 L of water to obtain 352.0 kg of chloromethyl hexafluoroisopropyl ether with a GC purity of 99.1% (the acetal impurity content was 0.8%) and a yield of 91.1%.

Embodiment 2

[0026] In a 1000L reactor, add 450kg sulfolane, 105kg potassium fluoride and 30kg pentaerythritol, then add 140kg chloromethyl hexafluoroisopropyl ether and 25kg purified water. Heated, reacted at 97-102°C for 10 hours, cooled down, added 150kg of purified water, distilled to obtain 105.0kg of crude sevoflurane, rectified to obtain 64.0kg of sevoflurane finished product, GC purity 99.991%.

Embodiment 3

[0027] Embodiment 3: according to US6100434 method

[0028] Add 50kg of aluminum trichloride to a 200L reactor, cool down to -5°C to 0°C, add 63kg of hexafluoroisopropanol dropwise under stirring, continue stirring for 0.5 hours after dropping, then add 12kg of paraformaldehyde, the reaction temperature Below 35°C, the reaction was continued for 17 hours. Lower the temperature below 0°C, add 100L of 6mol / l hydrochloric acid dropwise (solidification occurs during the process), and the temperature during the dropwise addition of hydrochloric acid should not exceed 15°C. The lower organic layer was washed twice with 100 L of water to obtain 69.9 kg of chloride with a GC purity of 87.0% (the acetal impurity content was 12%) and a yield of 86.1%.

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Abstract

The invention relates to a preparation method of chloromethyl hexafluoroisopropyl ether. Specifically, the present invention relates to a method for preparing chloromethyl hexafluoroisopropyl ether, wherein the solvent used in the reaction contains chloromethyl hexafluoroisopropyl ether. The preparation method introduces its own product as a solvent, which not only solves the solidification phenomenon of the reaction system during the reaction process, but also greatly improves the purity of the product, which is beneficial to industrial production.

Description

technical field [0001] The invention relates to a preparation method of chloromethyl hexafluoroisopropyl ether and a method for preparing sevoflurane through the preparation method. Background technique [0002] Sevoflurane (fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether) is a halogenated volatile anesthetic widely used in clinical. Chloromethyl hexafluoroisopropyl ether is an important intermediate for the synthesis of sevoflurane. [0003] [0004] US6100434 reports a method for preparing chloromethyl hexafluoroisopropyl ether in the presence of anhydrous aluminum chloride and paraformaldehyde using hexafluoroisopropanol as a raw material. We found that since no solvent is added during the reaction in this method, there is a solidification phenomenon in the reaction system during the preparation of chloromethyl hexafluoroisopropyl ether, especially in the process of industrial scale-up production. The solidification phenomenon is more obvious, and the reaction can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/01C07C41/22C07C43/12
CPCC07C41/01C07C41/22C07C43/123
Inventor 周庆海
Owner JIANGSU HENGRUI MEDICINE CO LTD
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