Purification of desflurane containing R-123

a technology of desflurane and r-123, which is applied in the field of purification of 2difluoromethoxy1, 1, 1, and 2tetrafluoroethane, can solve the problem of not being able to separate r-123 from desflurane by distillation

Active Publication Date: 2010-01-05
ULTRA MEK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since R-123 and desflurane have similar boiling points (27° C. ) and 23° C., respectively) it is not easy to separate the R-123 from the desflurane by distillation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example

[0018]To 28.5 kg of desflurane obtainable from the process described in Provisional Application Ser. No. 60 / 643,301 is added 2.5 kg of water. The mixture is then allowed to reflux for duration shown in the following table and both the overhead (O / H) and bottoms (B) samples are obtained and analyzed using GC.

[0019]

AfterRefluxingSampleHrs.DesfluraneR-123S / M—99.46%0.33%O / H7hrs.91.69%8.25%B7hrs99.97%168ppmO / H13hrs.92.63%7.32%B13hrs99.98%39ppmO / H16hrs.92.98%6.98%B16hrs99.99%21ppmO / H23hrs.94.89%5.08%B23hrs99.99%ppm

The column is locked off and drained, the material in the pot is distilled and fractions are collected after distilling 4 kg, 12 kg, 16 kg and 22 kg. These fractions are then analyzed using GC. Finally the total amount of material collected is analyzed. The results are shown in the table below.

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PUM

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Abstract

A process for preparing 2-difluoromethoxy-1,1,1,2-tetrafluoroethane (desflurane) comprising the following steps: (a) providing a first mixture comprising desflurane and 2,2-dichloro-1,1,1-trifluoroethane (R-123); (b) adding water to the first mixture to form a second mixture; and (c) fractionally distilling the second mixture to yield a desflurane product purer in R-123 than said the mixture. Also described is a purified desflurane product prepared by the process, and intermediate products comprising water added to a mixture of desflurane and R-123.

Description

BACKGROUND OF THE INVENTION[0001]1. Field of the Invention[0002]The present invention relates to the purification of 2-difluoromethoxy-1,1,1,2-tetrafluoroethane (desflurane), which is a well known inhalation anesthetic.[0003]2. Description of Related Art[0004]U.S. Provisional Application No. 60 / 643,301 describes a process for the preparation of desflurane by reaction of 2-chloro-2-difluoromethoxy-1,1,1-trifluoroethane (isoflurane) with hydrogen fluoride (HF) over a fixed bed catalysts. This process has a number of advantages in that it is greener than previous processes, highly efficient and adaptable to a continuous process.[0005]Even though this process also yields desflurane of a purity well within the specifications for anesthetic grade desflurane, the product contains a very small amount of 2,2-dichloro-1,1,1-trifluoroethane (R-123) as a by-product. Since R-123 and desflurane have similar boiling points (27° C. ) and 23° C., respectively) it is not easy to separate the R-123 fr...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): A61M15/00
CPCC07C41/44A61M2202/048
Inventor MAZZELL, PAULMURIN, PETER
Owner ULTRA MEK
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