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Novel crystal form cisatracurium besylate and crystallization method thereof

A technology of atracurium cis-benzenesulfonate and its crystal form, which is applied in the field of new crystal form of atracurium cis-benzenesulfonate and its crystallization, can solve problems such as difficult to reproduce, reduce usage and increase production Efficiency, good crystallization conditions and effect of purification method

Pending Publication Date: 2022-02-08
JIANGSU CHENGXIN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is too specific to be reproduced, and it is rare to use such a complex solvent system in a one-step crystallization operation

Method used

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  • Novel crystal form cisatracurium besylate and crystallization method thereof
  • Novel crystal form cisatracurium besylate and crystallization method thereof
  • Novel crystal form cisatracurium besylate and crystallization method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] This embodiment provides a crystallization method of atracurium cis-benzenesulfonate and the obtained new crystal form of atracurium cis-benzenesulfonate, the operation is as follows:

[0057] (1) 10.02 g (purity 98.56%) of the amorphous atracurium cis-benzenesulfonate solid after precipitating was stirred and dissolved with 10.00 g of acetone at 22° C.;

[0058] (2) Add the acetone solution obtained in step (1) dropwise into 80 mL of ethyl acetate solvent at 25° C. for crystallization, and stir at a speed of 210 rpm while adding dropwise, and the dropwise addition is completed in 50 minutes;

[0059] (3) After the dropwise addition, continue to grow crystals at 20°C and 75rpm under stirring conditions for 2h, then filter with suction to obtain a filter cake, vacuum dry at 25°C for 48h, collect the materials, and obtain atracurium cis-benzenesulfonate crystals 9.80g, the purity is 99.89%, and the yield is 99.12%.

[0060] The product that obtains is carried out HPLC de...

Embodiment 2

[0067] This embodiment provides a crystallization method of atracurium cis-benzenesulfonate and the obtained new crystal form of atracurium cis-benzenesulfonate, the operation is as follows:

[0068] (1) 10.03 g (purity 98.56%) of the amorphous atracurium cis-benzenesulfonate solid after precipitating was stirred and dissolved with 10.00 g of acetone at 25° C.;

[0069] (2) Add the acetone solution obtained in step (1) dropwise into 80 mL of ethyl acetate solvent at 25° C. for crystallization, and stir at a speed of 210 rpm while adding dropwise, and the dropwise addition is completed in 55 minutes;

[0070] (3) After the dropwise addition, continue to grow crystals at 25°C and 80rpm under stirring conditions for 2h, then filter with suction to obtain a filter cake, vacuum dry at 25°C for 48h, collect the materials, and obtain atracurium cis-benzenesulfonate crystals 9.86g, the purity is 99.85%, and the yield is 98.53%.

[0071] The obtained product was detected by XRD spectr...

Embodiment 3

[0073] This embodiment provides a crystallization method of atracurium cis-benzenesulfonate and the obtained new crystal form of atracurium cis-benzenesulfonate, the operation is as follows:

[0074] (1) 10.02 g (purity: 98.56%) of amorphous atracurium cis-benzenesulfonate solid after precipitating was stirred and dissolved at 18° C. with 10.00 g of acetone;

[0075] (2) Add the acetone solution obtained in step (1) dropwise into 100 mL of ethyl acetate solvent at 18° C. for crystallization, and stir at a speed of 220 rpm while adding dropwise, and the dropwise addition is completed in 58 minutes;

[0076] (3) After the dropwise addition, continue to grow crystals at 18°C ​​and 75rpm under stirring conditions for 2.5h, then filter with suction to obtain a filter cake, vacuum dry at 30°C for 30h, collect the materials, and obtain atracurium cis-benzenesulfonate Crystal 9.91g, purity 99.60%, yield 99.08%.

[0077] Carry out XRD spectrogram detection to the product that obtains,...

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Abstract

The invention relates to novel crystal form cisatracurium besylate and a crystallization method thereof. The crystallization method comprises the following steps of: dissolving amorphous cisatracurium besylate with acetone, adding the obtained solution into an ethyl acetate solvent, and crystallizing to obtain a cisatracurium besylate crystal. The crystallization method only relates to two organic solvents, namely acetone and ethyl acetate, the dosage is relatively small, the crystallization time is short, and the crystallization method is more suitable for industrial production from the angle of amplification. Meanwhile, the prepared novel crystal form cisatracurium besylate is very high in quality, the purity can reach 99.89%, the yield can reach 99.12%, and a very good crystallization condition and purification method for cisatracurium besylate are provided.

Description

technical field [0001] The invention belongs to the technical field of atracurium cis-benzenesulfonate purification, and in particular relates to a new crystal form of atracurium cis-benzenesulfonate and a crystallization method thereof. Background technique [0002] The chemical name of atracurium cis-benzenesulfonate is: (1R,1'R,2R,2'R)-2,2'-(3,11-dioxo-4,10-dioxtridecane Methylene) bis(1,2,3,4-tetrahydro-6,7-dimethoxy-2-methyl-1-veratrylisoquinoline) dibenzenesulfonate. [0003] Atracurium cis-besylate is a neuromuscular blocking agent developed by GlaxoSmithKline (GSK), trade name NimbexTM. Atracurium cis-besylate has the characteristics of being metabolized through non-hepatic and non-kidney pathways, and its muscle relaxant effect is 3 times stronger than that of atracurium besylate. It has the clinical advantages of quick onset, strong effect, rapid recovery, no release of histamine, little impact on cardiovascular, no accumulation, no muscle relaxant effect and no ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D217/20C07C309/29C07C303/44
CPCC07D217/20C07C309/29C07C303/44C07B2200/13
Inventor 李斌谭从祥魏云亮李二军祝俊张晨晨何宝亮李勇成
Owner JIANGSU CHENGXIN PHARMA
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