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A kind of method of recycling sevoflurane impurity f(1)

A technology of sevoflurane and impurities, applied in the field of recycling hexafluoroisopropyl chloromethyl ether, to achieve the effect of reducing environmental pollution and reducing costs

Active Publication Date: 2019-01-29
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, this method has the following technical problems: in the process of preparing the key intermediate hexafluoroisopropyl chloromethyl ether, sevoflurane impurity F(1) is produced, which is finally introduced into the crude sevoflurane with a content of about 5%

Method used

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  • A kind of method of recycling sevoflurane impurity f(1)
  • A kind of method of recycling sevoflurane impurity f(1)

Examples

Experimental program
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Effect test

Embodiment 1

[0019] In a three-necked flask equipped with a thermometer, a constant pressure dropping funnel, and a condenser, add 109.2 g of sevoflurane rectification residual liquid (containing 191.6%) and 80 g of aluminum trichloride, and mechanically stir to cool down to 5 ° C. Slowly add formaldehyde solution with a mass fraction of 50% (containing 30 g of formaldehyde (2) in total) while stirring, continue to stir and react for 3 h after adding, then slowly add 100 ml of 3 mol / L hydrochloric acid solution dropwise, let stand and separate, and use 3 mol / L for the organic layer. Wash with 100 ml of L sodium hydroxide solution, wash with water, stand to separate the layers, and collect the organic layer to obtain (3), with a purity of 93.2% and a mass yield of 88.9%.

Embodiment 2

[0021] In a three-necked flask equipped with a thermometer, a constant-pressure dropping funnel, and a condenser tube, add 105.1 g of sevoflurane rectification residual liquid (containing 195.1%) and 100 g of aluminum trichloride, and mechanically stir to cool to 5 ° C. While stirring, slowly add formaldehyde solution with a mass fraction of 50% (containing 45g of formaldehyde (2) in total), continue to stir and react for 6h after the addition is complete, then slowly add 150ml of 3mol / L hydrochloric acid solution dropwise, stand to separate and separate, and the organic layer is washed with 3mol / L Wash with 150 ml of L sodium hydroxide solution, wash with water, stand to separate layers, and collect the organic layer to obtain (3), with a purity of 89.2% and a mass yield of 89.5%.

Embodiment 3

[0023] In a three-necked flask equipped with a thermometer, a constant pressure dropping funnel and a condenser, add 116.8 g of sevoflurane rectification residue (containing 185.6%) and 80 g of aluminum trichloride, and mechanically stir to cool down to -5°C. While stirring, slowly add formaldehyde solution with a mass fraction of 50% (12g of formaldehyde (2) in total), continue to stir and react for 10h after adding, then slowly add 100ml of 3mol / L hydrochloric acid solution dropwise, let stand and separate, and use 3mol / L hydrochloric acid solution for the organic layer. Wash with 100 ml of / L sodium hydroxide solution, wash with water, stand to separate the layers, and collect the organic layer to obtain (3), with a purity of 88.9% and a mass yield of 83.7%.

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Abstract

The invention discloses a method for recycling a sevoflurane impurity F(1) in a sevoflurane coarse product to reduce the environment pollution. The method transforms a fluorine-containing effluent hard to degrade in the natural environment into a useful reagent, the environment pollution is reduced, the cost is lowered, and the clean production of sevoflurane is implemented.

Description

technical field [0001] The invention relates to the fields of organic chemistry and medicinal chemistry, in particular to a method for recovering hexafluoroisopropyl chloromethyl ether from sevoflurane synthesis waste liquid. Background technique [0002] Sevoflurane is a new inhalational anesthetic with rapid loss of consciousness and rapid recovery—ideal properties of contemporary anesthetics, and because of its mask-induced convenience and proven cardiovascular safety with minimal side effects, It has the advantages of not causing allergic reactions, etc., and has been widely used abroad. [0003] The currently reported synthetic route is mainly a novel method disclosed in US Patent No. 6,100,434 to prepare sevoflurane. Using hexafluoroisopropanol as the starting material, hexafluoroisopropyl chloromethyl ether is prepared through chloromethylation reaction, then fluorinated with potassium fluoride, and purified by rectification to obtain sevoflurane. The reaction route...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/28C07C41/34C07C43/12
CPCC07C41/28C07C41/34C07C43/123
Inventor 张贵民提文利王春燕
Owner LUNAN PHARMA GROUP CORPORATION