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Method for refining steroid muscle relaxant

A refining method and technology in the preparation process, which is applied in the refining field of steroid muscle relaxants, can solve the problems of difficult industrial production, complex operation, and high equipment requirements, and achieve the effects of simple and easy-to-obtain reagents, simple process, and improved purity

Active Publication Date: 2013-12-11
YICHANG HUMANWELL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adopts column chromatography and gradient cooling, which is complicated to operate, requires high equipment, and is not easy for industrial production.

Method used

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  • Method for refining steroid muscle relaxant
  • Method for refining steroid muscle relaxant
  • Method for refining steroid muscle relaxant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Mix 64g of vecuronium bromide, 120ml of water, and 4.5g of oxalic acid to obtain an aqueous solution of vecuronium bromide oxalate.

[0026] Wash the aqueous solution of vecuronium bromide oxalate with 300ml of dichloromethane, 100ml each time, for a total of 3 times. Extract the alkalized aqueous solution, collect and combine the dichloromethane extracts, dry with anhydrous sodium sulfate, filter, concentrate to a small volume, slowly drop into 640ml of anhydrous ether with stirring, filter, and dry to obtain vecuronium bromide 55.06g. The refined yield is 86%, and the HPLC purity is 99.6%.

Embodiment 2

[0028] Mix 64g of vecuronium bromide, 120ml of water, and 13.5g of oxalic acid to obtain an aqueous solution of vecuronium bromide oxalate.

[0029] The aqueous solution of vecuronium bromide oxalate was washed with 300ml of dichloromethane, 100ml each time, for a total of 3 times. Extract the alkalized aqueous solution with methane, collect and combine the dichloromethane extracts, dry with anhydrous sodium sulfate, filter, concentrate to a small volume, slowly drop into 640ml of anhydrous ether with stirring, filter, and dry to obtain vecuronium bromide 54.5g . The refined yield is 85%, and the HPLC purity is 99.5%.

Embodiment 3

[0031] Mix 64g of vecuronium bromide, 120ml of water, and 9g of oxalic acid to obtain an aqueous solution of vecuronium bromide oxalate.

[0032] Wash the aqueous solution of vecuronium bromide oxalate with 300ml of dichloromethane, 100ml each time, for a total of 3 times. Extract the alkalized aqueous solution, collect and combine the dichloromethane extracts, dry with anhydrous sodium sulfate, filter, concentrate to a small volume, slowly drop into 640ml of anhydrous ether with stirring, filter, and dry to obtain vecuronium bromide 56.33g. The refined yield is 88%, and the HPLC purity is 99.7%.

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Abstract

The invention discloses a method for refining a steroid muscle relaxant. The method for refining the steroid muscle relaxant comprises the following steps: firstly mixing the steroid muscle relaxant with water and acid to obtain an acidic salt aqueous solution, and washing by adopting an organic solvent A; then alkalifying the acidic salt aqueous solution, extracting the alkalified aqueous solution by adopting the organic solvent A, drying the collected extraction organic solvent A, filtering, concentrating to small volume, slowly dropping the concentrated organic solvent A into an organic solvent B, filtering, and drying to obtain a refined steroid muscle relaxant product. The method for refining the steroid muscle relaxant is simple in technology, good in controllability and strong in operability, industrialization production is easy to realize, only is once salifying alkalization operation needed, impurity content is obviously reduced, a better economic benefit during the industrialization production can be obtained, and production efficiency can be obviously improved.

Description

technical field [0001] The invention relates to a method for refining steroid muscle relaxants. Background technique [0002] Vecuronium bromide and rocuronium bromide are steroidal muscle relaxants, which are medium-acting non-depolarizing muscle relaxants, and act through competitive binding with acetylcholine receptors. It is mainly used as an auxiliary drug for general anesthesia, used for endotracheal intubation during general anesthesia and muscle relaxation during surgery. Rocuronium bromide is a steroidal non-depolarizing muscle relaxant, and its synthesis method and use are disclosed in European Patent EP0287150. WO0044334 discloses a compound injection composed of rocuronium bromide and other traditional muscle relaxants. The parenteral administration composition of US5767112 rocuronium bromide contains a muscle relaxant and a zwitterionic substance with a weight ratio of 2-30% and an isoionic point not greater than 7, and the pH value of the composition is 5.2-5...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J43/00
Inventor 张庆赵红卫汪淼郑华章田峦鸢李仕群郑炜李莉娥徐华斌晏涛
Owner YICHANG HUMANWELL PHARMA
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