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Preparation method of isoflurane

A technology of isoflurane and trifluoroethanol, which is applied in the field of preparation of 1-chloro-2, organic compounds, can solve the problems of high impurity content in the final product, difficulty in ensuring the yield of isoflurane, and difficulty in achieving repeated rectification, etc. Achieve the effects of easy quality control, improved yield and stable operation

Active Publication Date: 2006-09-27
LUNAN PHARMA GROUP CORPORATION
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the range of reaction conditions in this route is too wide, it is difficult to ensure the yield of isoflurane, and the impurity content of the final product is relatively high, and repeated rectification is also difficult to meet the requirements of the standard.

Method used

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  • Preparation method of isoflurane
  • Preparation method of isoflurane
  • Preparation method of isoflurane

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: the preparation of 2,2,2-trifluoroethyl difluoromethyl ether

[0020] Add 200g of TFE and 80g of NMP into the autoclave, close the autoclave, start stirring, add 173g of Freon-22 (F-22), then fill the autoclave with nitrogen, add 368g of 50% NaOH aqueous solution at 5°C under stirring, and control The temperature in the autoclave is between 36°C, after the addition, fill the autoclave with nitrogen to 18-20kg / cm 2 , stirred for 3 hours. Transfer the reaction solution in the still to the distillation still, heat and fractionate in a water bath with stirring, collect fractions below 30°C to obtain CF 3 CH 2 OCHF 2 180g, the residue continued to distill, reclaimed TFE60.5g, conversion rate was 60%, and yield was 86% (according to the TFE consumption calculation).

Embodiment 2

[0021] Embodiment 2: the preparation of isoflurane

[0022] Put 300g (2.0mol) 2,2,2-trifluoroethyl difluoromethyl ether into the chlorination tank, turn on the stirring and fluorescent lamp, and feed a small amount of chlorine gas. When the color of the chlorine gas in the tank disappears, use a gas flow meter to control The speed of passing chlorine gas makes it react completely without overflowing. The water bath controls the reaction temperature at 15-20° C., feeds 0.9 mol of chlorine gas, and then reacts at 15-20° C. for 30 minutes. The reaction liquid was distilled, and the fraction below 40°C was collected as the etherified product to obtain 150 g. Cool the residue to 5-10°C, slowly add sodium hydroxide solution dropwise under stirring, stir for 10 minutes after adding, let stand for 10 minutes, put the lower layer chloride solution into the storage tank, wash it with water three times, and remove the lower layer chloride solution The solution was put into a drying tan...

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Abstract

A process for preparing isolfuothane from trifluoroethanol, N-methypyrrolidone and freon-22 includes such steps as etherifying and chloridizing.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a preparation method of 1-chloro-2,2,2-trifluoroethyl difluoromethyl ether (ie isoflurane), and belongs to the field of medicine and chemical industry. Background technique [0002] Isoflurane is a general inhalational anesthetic and is the isomer of enflurane. Animal experiments and clinical studies have shown that isoflurane has low biochemical transformation, low liver and kidney toxicity, small circulation inhibition, good muscle relaxation, rapid and stable induction and recovery, no spasmodic brain waves, good recovery and small side effects, etc. advantage. [0003] There are many preparation methods of isoflurane reported in the literature, but the process conditions are relatively complicated, the synthesis route is long, and the cost is high. U.S. Patent US3535425 (1970) discloses a kind of preparation method of isoflurane, and its reaction route is: [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/12C07C41/01
Inventor 赵志全
Owner LUNAN PHARMA GROUP CORPORATION
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