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Synthesis method of desflurane

A synthetic method, the technology of desflurane, applied in the field of medicine and chemical industry, can solve the problems of slow reaction rate, low reaction temperature, easy explosion, etc.

Inactive Publication Date: 2012-08-01
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the preparation of desflurane by the reaction of hydrogen fluoride, fluorine gas and isoflurane is difficult to achieve industrialization because of its slow reaction rate, low reaction temperature and expensive reagents, and because fluorine gas and partially fluorinated carbon Mixture of hydrogen compounds is explosive; bromine trifluoride is used for fluorination, because bromine trifluoride is a highly toxic and dangerous substance, it will explode when it comes in contact with water or organic matter, and it is difficult to operate; while potassium fluoride is used for fluorination Then the risk of the synthetic route introduced above can be avoided. Potassium fluoride is cheap, stable in physical properties, much less toxic than bromine trifluoride and hydrogen fluoride, and easy to operate, but the low yield is not conducive to industrial production.

Method used

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  • Synthesis method of desflurane
  • Synthesis method of desflurane
  • Synthesis method of desflurane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Fluorination of 1-chloro-2,2,2-trifluoroethyl difluoromethyl ether

[0030] Add 144ml of diethylene glycol, 39.79g of dry potassium fluoride into the autoclave, add 66.46g of isoflurane, seal and stir, heat up to 220-230°C, and react for 10-12 hours. After the reaction, put the autoclave in Cool at room temperature overnight, and then circulate the refrigerated liquid into the autoclave to cool down. After about 4 hours, until the pressure no longer drops, open the autoclave, pour the reaction solution and residue into a round bottom flask, heat and distill, and condense with the refrigerated liquid The condenser was refluxed, and fractions were collected to obtain 29.9 g of a crude product of desflurane, with a GC content of 88.63% and a yield of 43.8%.

Embodiment 2

[0031] Example 2: Purification of 1-chloro-2,2,2-trifluoroethyl difluoromethyl ether

[0032] Use a rectification column to rectify 61.7g of crude desflurane product with a GC content of 85%. ℃, the receiving bottle was kept warm in an ice-salt bath in a self-made vacuum flask. At first, it was controlled to be in a total reflux state, and the fractions were collected after a continuous reflux was formed. The reflux ratio was controlled to be 1:1. The collected desflurane distillation product was 42g, with a GC content of 99.89% and a distillation yield of about 80%. The distillation residual liquid can be recycled in the next batch.

[0033] 1HNMR (400MHz, CDC13) δ: 6.42(t, 1H, -CH), 5.90(d, 1H, -CH).

[0034] 19FNMR (367.5MHz, CDC13) δ: -85.10 (s, 3F, -CF3), -85.76 (d, 1F, -CF, J=157.65), -87.20 (d, 1F, -CF, J=157.65), -146.91(s, 1F, -CF).

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Abstract

The invention provides a synthesis method of desflurane. According to the synthesis method, 1-chlorine-2,2,2-trifluoride ethyl difluoro methyl ether (isoflurane) is used as raw materials, 2-difluoro methyl-1,1,1,2-tetrafluoroethane (desflurane) is obtained through fluorination reaction, and the yield reaches 43.8 percent. The yield is further improved on the basis of the prior art, the cost is reduced, the purity of products is improved, the operability is enhanced, and the synthesis method is suitable for industrialized production.

Description

Technical field: [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing 2-difluoromethyl-1,1,1,2-tetrafluoroethane, and belongs to the field of medicine and chemical industry. Background technique: [0002] Desflurane is a fluorine-containing inhalation anesthetic that was launched in the market in 1992. It is a fluorinated chlorine compound of isoflurane. It has a lower boiling point (23°C) and a blood / gas partition coefficient of 0.42, which is lower than other fluorine-containing inhalation anesthetics. , so the induction and recovery of anesthesia are fast, easy to adjust the depth of anesthesia. Its minimum intraalveolar concentration (MAC) is 5.6% to 6%, so the anesthetic effect is also lower than others. It has less impact on the circulatory system than other inhaled anesthetics, and has no damage to liver and kidney functions. Another advantage is that it can be in contact with soda lime. Desflurane ...

Claims

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Application Information

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IPC IPC(8): C07C43/12C07C41/22
Inventor 吴范宏叶文涛赵敏王琼沈刚
Owner EAST CHINA UNIV OF SCI & TECH