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Industrial preparation method of dexmedetomidine hydrochloride

A technology for dexmedetomidine hydrochloride and dexmedetomidine, which is applied in the field of medicine, can solve problems such as corrosion, rust, toxicity and low yield in workshops and equipment, and achieves avoiding health hazards, reducing process steps, and reducing yield. High rate and purity effect

Inactive Publication Date: 2017-04-26
江苏开元医药有限公司
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0007] The raw materials of this reaction route are easy to get, the price is low, but the yield is low, and the chlorinated reagent thionyl chloride used in the reaction process is poisonous, strong corrosion, easy to damage the health of the operator, and easily cause damage to the workshop and equipment. Corrosion, rust, etc.

Method used

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  • Industrial preparation method of dexmedetomidine hydrochloride
  • Industrial preparation method of dexmedetomidine hydrochloride
  • Industrial preparation method of dexmedetomidine hydrochloride

Examples

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Embodiment 1

[0045] (1) Preparation of medetomidine

[0046] Into a 20L dry glass reactor, add 1.86kg of trimethylsilimidazole and 9.85L of dichloromethane in sequence, stir for 10 minutes, start to add 2.52kg of titanium tetrachloride dropwise, control the internal temperature at 20-30°C, continue stirring after dropping After 30 minutes, continue to add 1.33 kg of 1-(2,3-dimethylbenzene) ethanol dropwise under the temperature adjustment. After the drop is completed, continue to stir and react for 18 hours, and take samples for TLC detection or HPLC detection. After the reaction is completed, add the reaction solution into 10L of ice water, stir for 20min, let stand to separate layers, separate the aqueous phase and the organic phase, discard the organic phase, adjust the pH value of the aqueous phase to 10 with sodium hydroxide, add 12L of dichloromethane for extraction , separated the organic phase, added 4L dichloromethane to the aqueous phase for extraction, and combined the organic p...

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Abstract

The invention discloses an industrial preparation method of dexmedetomidine hydrochloride, and belongs to the field of medicines. The method comprises the following steps: directly carrying out a Friedel-Crafts alkylation reaction on initial raw materials comprising 1-(2,3-dimethylphenyl)ethanol not subjected to a chlorination (thionyl chloride) reaction and protected imidazole under the catalysis of a Lewis acid to obtain racemic dexmedetomidine, carrying out pre-resolution purification on the racemic dexmedetomidine through a chiral acid, carrying out chiral acid resolution and alkali dissociation, and adding a hydrochloric acid organic solvent to form a salt in order to obtain the dexmedetomidine hydrochloride. The method avoids use of the toxic and corrosive regent thionyl chloride, allows the above product with high chiral and chemical purity to be obtained and the yield to be high, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicine, in particular to a preparation method of high-purity chiral drugs, in particular to a simple industrial preparation method for obtaining high-purity dexmedetomidine hydrochloride. Background technique [0002] Dexmedetomidine Hydrochloride, chemical name: (+)-4-(S)-[1-(2,3-dimethylphenyl)ethyl]-1H-imidazole hydrochloride, The structure is as follows: [0003] [0004] This product is an α2-adrenergic receptor agonist, used for sedation during tracheal intubation and mechanical ventilation in surgical patients undergoing general anesthesia. Dexmedetomidine hydrochloride was first launched in the United States in March 2000 (trade name Precedex), and was subsequently approved for marketing in many countries. At present, many domestic pharmaceutical companies have imitated it and put it on the market. [0005] Dexmedetomidine hydrochloride is obtained by splitting its racemic form, dexmedetomidine. The...

Claims

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Application Information

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IPC IPC(8): C07D233/58
CPCC07D233/58
Inventor 燕立波赵纪山李佼佼金永华王军花杨振伟
Owner 江苏开元医药有限公司
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