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A kind of purification method of sevoflurane

A purification method, the technology of sevoflurane, which is applied in the field of separation and purification of chemicals, can solve the problems of increasing production cost and complexity, and the separation effect is not very good, and achieves the effect of simple method and easy realization

Active Publication Date: 2017-07-18
HUADONG MEDICINE XIAN BODYGUARD PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned methods have not only increased the production cost and complexity, but the separation effect is not very good, and there are also environmental protection problems.

Method used

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  • A kind of purification method of sevoflurane
  • A kind of purification method of sevoflurane
  • A kind of purification method of sevoflurane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Using hexafluoroisopropanol and paraformaldehyde as raw materials, the crude product of sevoflurane was prepared by fluorination with potassium fluoride after the reaction under the catalysis of aluminum trichloride. After testing, the crude product of sevoflurane contained hexafluoroisopropanol , and other by-product impurities such as methyl hexafluoroisopropyl ether, chloromethyl hexafluoroisopropyl ether, chloromethyl-1,1,3,3,3-pentafluoro-2-propenyl ether, Polyether formed from fluoromethyl-1,1,3,3,3-pentafluoro-2-propenyl ether, hexafluoroisopropanol and paraformaldehyde [(CF 3 ) 2 CH(CH 2 O) n OCH(CF 3 ) 2 ] and some other unknown impurities.

[0024] The prepared crude sevoflurane is purified. The purification method includes: adding the crude sevoflurane to be purified into the rectification tank of the rectification tower for rectification and purification. The temperature of the rectification tank is 63 ° C, so that the crude sevoflurane Boil and reflux...

Embodiment 2

[0027] Purify the crude sevoflurane in Example 1. The purification method includes: adding the crude sevoflurane to be purified into the rectification tank of the rectification tower for rectification and purification. The temperature of the rectification tank is 65 ° C, making seven The crude halothane boils and refluxes in the rectification column. After the reflux reaches a stable level, control the reflux ratio to 5:1. Collect the previous fraction from the top of the rectification column. When the temperature at the top of the rectification column reaches 57°C, reduce the reflux ratio to 3. : 1, collect the positive fraction from the top of the rectification tower to obtain purified sevoflurane, and stop collecting when the temperature at the top of the rectification tower drops to 50°C; the rectification column is filled with stainless steel θ ring fillers with embedded silica gel , the stainless steel θ ring packing with embedded silica gel includes a stainless steel θ r...

Embodiment 3

[0031]Purify the crude sevoflurane in Example 1. The purification method includes: adding the crude sevoflurane to be purified into the rectification tank of the rectification tower for rectification and purification. The temperature of the rectification tank is 60 ° C, making seven The halothane crude product boils and refluxes in the rectification column. After the reflux reaches a steady state, control the reflux ratio to 3:1. Collect the front fraction from the top of the rectification column. When the temperature at the top of the rectification column reaches 53°C, reduce the reflux ratio to 2. : 1, collect the positive fraction from the top of the rectification tower to obtain purified sevoflurane, and stop collecting when the temperature at the top of the rectification tower drops to 50°C; the rectification column is filled with stainless steel θ ring fillers with embedded silica gel , the stainless steel θ ring packing with embedded silica gel includes a stainless steel...

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Abstract

The invention discloses a purification method of sevoflurane. The method comprises steps as follows: a coarse sevoflurane product to be purified is added to a rectifying still of a rectifying column for rectifying purification, the reflux ratio is controlled to be (3-5):1 after reflux is stabilized, a front fraction is collected from the top end of the rectifying column, the reflux ratio is decreased to (1-3):1 when the rectifying column top temperature is 53-57 DEG C, a positive fraction is collected from the top end of the rectifying column, purified sevoflurane is obtained, and collection is stopped when the rectifying column top temperature is decreased to 50 DEG C; the rectifying column is filled with stainless steel theta ring packing or stainless steel theta ring packing embedded with silica gel, and a silica gel column is connected below the rectifying column filled with the stainless steel theta ring packing in series. Silica gel is introduced, the adsorption of silica gel to hexafluoroisopropanol impurities is utilized, the distil-off time of hexafluoroisopropanol can be well delayed, and sevoflurane is effectively separated from common impurities and stubborn hexafluoroisopropanol impurities through control on the temperature of the rectifying still and the reflux ratio.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of chemicals, and in particular relates to a method for purifying sevoflurane. Background technique [0002] Sevoflurane, chemical name: fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether, first approved for marketing in the United States in 1955, is an inhalation anesthesia for induction and maintenance of general anesthesia medicine. [0003] Among the many known methods for preparing sevoflurane, the most commonly used method is to use hexafluoroisopropanol (HFIP) and paraformaldehyde as raw materials, react under the catalysis of aluminum trichloride, and then react with potassium fluoride chemical preparation. However, unreacted hexafluoroisopropanol (HFIP) and methyl hexafluoroisopropyl ether (MHFIP), chloromethyl hexafluoroisopropyl ether, chloromethyl-1,1,3 ,3,3-pentafluoro-2-propenyl ether, fluoromethyl-1,1,3,3,3-pentafluoro-2-propenyl ether, hexafluoroisopropanol a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/36C07C41/42C07C43/12
CPCC07C41/36C07C41/42C07C43/12
Inventor 袁民政薛锋锋侯海婷
Owner HUADONG MEDICINE XIAN BODYGUARD PHARMA CO LTD
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