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Method for purifying atracurium besylate by two-phase extraction

Atracurium besylate, extraction technology, applied in the direction of organic chemistry, etc., can solve the problems of high residue, unsatisfactory effect, affecting the clinical drug safety of products, etc., and achieves reduction of purification costs, significant social benefits and economic effect

Active Publication Date: 2009-01-07
JIANGSU HENGRUI MEDICINE CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The synthetic route of atracurium besylate is relatively simple, but because of the use of highly toxic substances such as toluene and methyl benzenesulfonate in the reaction and purification process, and these highly toxic substances have high residues in the final product, significantly Affect the clinical drug safety of the product
At present, multiple recrystallizations of toluene are often used to minimize the residue of methyl benzenesulfonate in the final product, but the results are not ideal

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] Example 1 Method for purifying atracurium besylate by two-phase extraction

[0018] Add 100ml of acetonitrile and an appropriate amount of water to 500g of atracurium benzenesulfonate crude product. After dissolving, add benzenesulfonic acid to adjust the pH of the solution to 3-4, and control the final volume of the obtained acidic solution to 3L; first extract the acidic solution with toluene. Solution 2 times, the amount of toluene used for each extraction is 2L, discard the toluene extract; then use 2L to form ethyl acetate: n-hexane (5: 1) mixed solvent to extract the acidic solution once, discard the mixed extract; Then, extract the acidic solution with dichloromethane for 3 times, the amount of dichloromethane used for each extraction is 1.5 L, combine the extracts of 3 times of dichloromethane, add magnesium sulfate to dry and dehydrate, concentrate, add diethyl ether to carry out eluting crystallization, Filtrate and vacuum dry overnight to obtain 430g of pu...

Embodiment 2

[0019] Example 2 Method for purifying atracurium besylate by two-phase extraction

[0020] Add water to dissolve 500g of atracurium benzenesulfonate crude product, add benzenesulfonic acid to adjust the pH of the solution to 3-4 water and control the final volume of the resulting acidic solution to 4L; first extract the aqueous solution twice with n-hexane, each extraction The amount of n-hexane used is 2L, and the n-hexane extract is discarded; the acidic solution is extracted once with a mixed solvent of ethyl acetate:n-hexane (5:1) with 2L, and the mixed extract is discarded; then, extracted with chloroform The acidic solution was used 3 times, and the amount of chloroform used for each extraction was 1.5 L. The chloroform extracts were combined for 3 times, dried and dehydrated by adding magnesium sulfate, concentrated, and washed by adding a mixed solvent consisting of ethyl acetate:n-hexane (5:1). Crystallization, filtration, and vacuum drying overnight to obtain 425...

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PUM

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Abstract

The invention relates to a novel method for purifying atracurium besylate atracurium besilate, which utilizes a two-phase extraction method to separate and remove methyl benzene sulfonate which remains in atracurium besylate atracurium besilate, and toluene is not used during the purification process, so the residual quantity of toxic solvent in atracurium besylate atracurium besilate can be effectively controlled and obviously reduced, and the drug safety thereof is increased obviously.

Description

technical field [0001] The invention relates to a method for purifying atracurium besylate by a two-phase extraction method, and the obtained atracurium besylate has extremely low residual amount of methyl besylate. Background technique [0002] Atracurium besylate was developed by the British Glaxo welcome company and was launched in the UK in 1996. It is a non-depolarizing muscle relaxant. It has the same effect as tubocurarine, but its potency is 2.5 times that of tubocurarine. It has the characteristics of quick onset, short duration of action, no effect on heart, liver, kidney function and no accumulation of therapeutic dose, etc. It is widely used clinically to prevent and treat various situations that require muscle relaxation or control of breathing. [0003] The synthetic route of atracurium besylate is relatively simple, but because of the use of highly toxic substances such as toluene and methyl benzenesulfonate in the reaction and purification process, and these ...

Claims

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Application Information

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IPC IPC(8): C07D217/04
Inventor 孙飘扬陈永江郁光亮
Owner JIANGSU HENGRUI MEDICINE CO LTD
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