Preparation of furane used as inhalation anesthetic

A technology of isoflurane and anesthetic, applied in the field of preparation of isoflurane, can solve the problems of high risk, high cost, low conversion rate, etc., and achieve the effect of low risk, low cost and small impurity content

Inactive Publication Date: 2009-06-24
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] The purpose of the present invention is to provide a method for preparing isoflurane used as an inhal...

Method used

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  • Preparation of furane used as inhalation anesthetic
  • Preparation of furane used as inhalation anesthetic
  • Preparation of furane used as inhalation anesthetic

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) 150gCCl 4 Add it into the reaction vessel, cool it in an ice bath to 0-5°C, add 135g (1mol) of anhydrous AlCl 3 , after stirring for 30 minutes, start to add 150gHFE (1mol) dropwise, control the drop rate, and keep the temperature in the system at 0-5°C; after the addition is completed, keep 20-40°C to continue the reaction for 24h;

[0032] (2) Cool the reaction product to 0-5°C, slowly add 333ml of 6mol / L hydrochloric acid dropwise, and leave to separate to obtain an oil phase;

[0033] (3) The oil phase is washed with 100ml of 2% sodium hydroxide solution, then washed with water (50 × 3ml) to neutrality, added anhydrous calcium chloride to dry, and after 24h, it is rectified with a 120 × 3cm packed column, 148 g of fractions at 42-48°C were collected and analyzed by MS-GC. The isoflurane content was 96.56%, and the yield was 77.5%.

Embodiment 2

[0035] (1) 150gCCl 4 Add it into a 500ml three-neck flask, cool it in an ice bath to 0-5°C, add 106.6g (0.8mol) of anhydrous AlCl 3 , after stirring for 35 minutes, start to add 150gHFE (1mol) dropwise, control the drop rate, keep the temperature in the system at 0-5°C, and keep the temperature at 20-40°C to continue the reaction for 12h after the addition is completed;

[0036] (2) Cool the reaction product to 0-5°C, slowly add 250ml of 6mol / L hydrochloric acid dropwise, and leave to separate to obtain an oil phase;

[0037] (3) The oily phase was washed with 100ml of 1% sodium hydroxide solution, then washed with water (50×3ml) until neutral, added anhydrous calcium chloride to dry, and after 12h, it was rectified with a 120×4cm packed column, and collected 137.4 g of fractions at 42-48°C were analyzed by MS-GC, the isoflurane content was 96.46%, and the yield was 73.6%.

Embodiment 3

[0039] (1) 300gCCl 4 Add it to a 1000ml three-necked flask with a reflux condenser, cool it to 0°C in an ice bath, and add 270 (2mol) of anhydrous AlCl 3 , after stirring for 25 minutes, start to add 150g HFE (1mol) dropwise, control the drop rate, keep the temperature in the system at 0-5°C, and keep the temperature at 20-40°C to continue the reaction for 24h after the addition is completed;

[0040] (2) Cool the reaction product to 0-5°C, slowly add 667ml of 12mol / L hydrochloric acid dropwise, and leave to separate to obtain an oil phase;

[0041] (3) The oil phase is washed with 200ml of 2% sodium hydroxide solution, then washed with water (100 × 3ml) to neutrality, added anhydrous calcium chloride to dry, and after 24h, it is rectified with a 120 × 3cm packed column, 142.4 g of fractions at 42-48°C were collected and analyzed by MS-GC. The isoflurane content was 96.42%, and the yield was 76.3%.

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Abstract

The invention belongs to the technical field of medicine and chemical engineering and in particular relates to a preparation method of isoflurane for inhalation anesthetics. The method solves the problem that the conversion rate is low, the cost is high and the fatalness is high in the prior art; in order to overcome the problems in the prior art, the technical proposal is as follows: the preparation method of isoflurane for inhalation anesthetics comprises the following steps in sequence: (1)reaction: HFE with water content less than 50ppm and lewis acid which are taken as raw materials to take reaction according to the mole number ratio of 1:0.8-3; (2) hydrochloric acid is dropwise added, the mixture stands for layer separation and then oil phase is obtained; (3) the isoflurane product is obtained by neutralizing, washing and rectifying the oil phase. Compared with the prior art, the method has the advantages of high yield, low cost, low hazard and convenient separation and purification.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a preparation method of isoflurane used as an inhalation anesthetic. Background technique [0002] Isoflurane (CF 3 CHClOCF 2 H) is a systemic inhalation anesthetic, which is an isomer of enflurane. Isoflurane has low biochemical transformation, low toxicity to liver and kidney, small circulation inhibition, rapid and smooth induction and recovery, and no spasmodic cerebral palsy. Radio waves, good recovery and less side effects. [0003] The preparation method of isoflurane is more at present, but all exists weak point, describe respectively as follows: [0004] One, the patent US3535425 (1970) discloses a kind of preparation method of isoflurane, and its reaction scheme is: [0005] [0006] This route process is complicated, and synthetic route is long, wherein raw material dimethyl sulfate toxicity is bigger, and HF has stronger corro...

Claims

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Application Information

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IPC IPC(8): C07C43/12C07C41/22A61P23/00
Inventor 杨刚柴华张文庆杨会娥
Owner 中国中化股份有限公司
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