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Cisatracurium besylate with new crystal form and purifying method thereof

Atracurium cissulfonate and a purification method are applied in the field of new crystal form atracurium cissulfonate and its purification, which can solve the problems of difficulty in reproduction and the like, and achieve good stability and purification method. simple effect

Inactive Publication Date: 2017-11-17
江苏海悦康医药科技有限公司
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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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  • Cisatracurium besylate with new crystal form and purifying method thereof
  • Cisatracurium besylate with new crystal form and purifying method thereof
  • Cisatracurium besylate with new crystal form and purifying method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A new crystal form of atracurium cis-benzenesulfonate and its purification method, comprising the following steps:

[0034] (1) Preparation of amorphous atracurium cis-benzenesulfonate: Add 700mL of acetonitrile to a 2L reaction flask, stir, add 140g of crude atracurium cis-benzenesulfonate at 10±2°C, stir for 30-60min; filter , collect the filtrate; slowly add the filtrate into a 5L reaction flask containing 2800mL ether, stir and crystallize at 10±2°C for 6h; filter with suction, and wash the filter cake with 200mL ether; dry the filter cake at 35°C for 8h under reduced pressure, 100 g of white solid was obtained, namely amorphous atracurium cis-benzenesulfonate, with a yield of 71% and a purity of 93.3%. The XRPD pattern of amorphous cis-benzenesulfonate atracurium is shown in figure 1 shown.

[0035] (2) Preparation of new crystal form of atracurium cis-benzenesulfonate, including the following steps:

[0036] A. Dissolve 2.0 g of amorphous atracurium cis-benzene...

Embodiment 2

[0041] A new crystal form of atracurium cis-benzenesulfonate and its purification method, comprising the following steps:

[0042] (1) Preparation of amorphous atracurium cis-benzenesulfonate: Add 700mL of acetonitrile to a 2L reaction flask, stir, add 140g of crude atracurium cis-benzenesulfonate at 10±2°C, stir for 30-60min; filter , collect the filtrate; slowly add the filtrate into a 5L reaction flask containing 2800mL ether, stir and crystallize at 10±2°C for 6h; filter with suction, and wash the filter cake with 200mL ether; dry the filter cake at 35°C for 8h under reduced pressure, 100 g of white solid was obtained, namely amorphous atracurium cis-benzenesulfonate, with a yield of 71% and a purity of 93.3%. The XRPD pattern of amorphous cis-benzenesulfonate atracurium is shown in figure 1 shown.

[0043] (2) Preparation of new crystal form of atracurium cis-benzenesulfonate, including the following steps:

[0044] A. Dissolve 1.0 g of amorphous atracurium cis-benzene...

Embodiment 3

[0049] A new crystal form of atracurium cis-benzenesulfonate and its purification method, comprising the following steps:

[0050] (1) Preparation of amorphous atracurium cis-benzenesulfonate: Add 700mL of acetonitrile to a 2L reaction flask, stir, add 140g of crude atracurium cis-benzenesulfonate at 10±2°C, stir for 30-60min; filter , collect the filtrate; slowly add the filtrate into a 5L reaction flask containing 2800mL ether, stir and crystallize at 10±2°C for 6h; filter with suction, and wash the filter cake with 200mL ether; dry the filter cake at 35°C for 8h under reduced pressure, 100 g of white solid was obtained, namely amorphous atracurium cis-benzenesulfonate, with a yield of 71% and a purity of 93.3%. The XRPD pattern of amorphous cis-benzenesulfonate atracurium is shown in figure 1 shown.

[0051] (2) Preparation of new crystal form of atracurium cis-benzenesulfonate, including the following steps:

[0052] A. Dissolve 1.0 g of amorphous atracurium cis-benzene...

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Abstract

The invention discloses cisatracurium besylate with a new crystal form and a purifying method thereof. The purifying method comprises the following steps: (A) adding amorphous cisatracurium besylate into a polar solvent with the volume being 20-40 times of that of the amorphous cisatracurium besylate, and stirring till being completely dissolved; (B) filtering the obtained solution by a microporous filtering membrane, then putting filtrate at the temperature of 22+ / -5 DEG C, stirring for 5-30 hours; and (C) filtering to obtain filtering cakes, carrying out vacuum drying for 2-14 hours at the temperature of 30-40 DEG C to obtain white powder. The cisatracurium besylate and the purifying method disclosed by the invention have the advantages that 2theta in an X-ray diffraction pattern has main characteristic diffraction peaks at 7.0+ / -0.2, 8.6+ / -0.2, 11.2+ / -0.2, 12.8+ / -0.2, 17.4+ / -0.2, 18.5+ / -0.2, 19.4+ / -0.2, 20.8+ / -0.2 and 23.9+ / -0.2; the stability is better, and the storage and transportation of crude drugs are convenient; and the purifying method is simple and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of purification of atracurium cis-benzenesulfonate, in particular to a new crystal form of atracurium cis-benzenesulfonate and a purification 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-dioxotridecane Methylene) bis(1,2,3,4-tetrahydro-6,7-dimethoxy-2-methyl-1-veratrylisoquinoline) dibenzenesulfonate, the chemical structure is as follows: [0003] Cisatracurium Besilate, a neuromuscular blocker developed by GlaxoSmithKline (GSK), trade name Nimbex TM . The drug was launched in the UK in 1996 and is used for surgery and other operations and intensive care treatment. As an adjunct to general anesthesia or as a sedative in the intensive care unit (ICU). [0004] US5453510 was the first to provide the synthetic method of atracurium cis-benzenesulfonate, and obtained a product with an isomer purity of 99% through p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D217/20
CPCC07D217/20C07B2200/13
Inventor 李惠裴欣宇姜春阳
Owner 江苏海悦康医药科技有限公司
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