Method for synthesizing sugammadex sodium through microwave reaction

A technology of sugammadex sodium and microwave reaction, which is applied in the field of microwave reaction synthesis of sugammadex sodium, can solve the problems of increasing the difficulty of industrial application and cumbersome processing process, and achieve good economy, simple follow-up purification and high product purity Effect

Inactive Publication Date: 2018-12-04
HEFEI BOSIKC PHARMTECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the processing process is relatively cumbersome, and the ion resin ne

Method used

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  • Method for synthesizing sugammadex sodium through microwave reaction
  • Method for synthesizing sugammadex sodium through microwave reaction
  • Method for synthesizing sugammadex sodium through microwave reaction

Examples

Experimental program
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Example Embodiment

[0032] Example 1:

[0033] Synthesis of Crude Sodium Gluconate of Shu Geng

[0034] Put sodium hydroxide (23.5g, 588mmol) into the reaction flask, add 150ml of water to dissolve completely; add 3-mercaptopropionic acid aqueous solution (39.0g, 368mmol, dissolved in 80ml of water) into the flask with stirring, add 6-deoxy- 6-Periodo-γ-cyclodextrin (40g, 18.4mmol), after the addition, put it in a microwave reactor and react for 30 minutes under 500w microwave radiation; after the reaction is complete, cool to room temperature, add 700mL DMF under stirring to crystallize, Filter, collect the solid, vacuum dry 45g of off-white solid with a purity of 98.33% (see attached Figure 3-4 ).

Example Embodiment

[0035] Example 2:

[0036] Purification of Sodium Gluconate

[0037] Under the protection of nitrogen, take 40g of crude Sodium Gluconate and dissolve it in a mixed solution of 100ml of water and 600ml of ethanol, stir and warm up to 40°C and drop to room temperature. A white solid is precipitated out and filtered with suction to obtain 35g of a white solid. The solid is tested by HPLC, and the purity is 99.82%, which meets the requirements of Shugan Sodium Gluconate API (see attached Figure 5-6 ).

Example Embodiment

[0038] Example 3:

[0039] Synthesis of Crude Sodium Gluconate of Shu Geng

[0040] Put sodium carbonate (15.9g, 150mmol) into the reaction flask, add 75ml water and 115ml N,N-dimethylformamide; add 3-mercaptopropionic acid aqueous solution (19.5g, 184mmol, dissolved in 80ml In water), add 6-deoxy-6-periodo-γ-cyclodextrin (40g, 18.4mmol), after the addition, put it in a microwave reactor and react under 300w microwave radiation for 60 minutes; after the reaction is complete, cool to room temperature , Add 400mL DMF under stirring to crystallize, filter, collect the solid, and vacuum dry to obtain 40g off-white solid with a purity of 98.26%

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Abstract

The invention belongs to the field of pharmacy, and especially relates to a method for synthesizing sugammadex sodium through microwave reaction. The method firstly provides that sugammadex sodium canbe prepared in a water-containing system; organic solvents like N,N-dimethylformamide used by traditional methods can be replaced in whole or in part by adopting water or a combination of the water and an organic solvent as a reactive solvent; and therefore, disadvantages of hard recovery, large pollution and high environmental protection costs caused by large amount of high boiling organic solvents can be improved. The sugammadex sodium can be rapidly synthesized by taking 3-mercaptopropionic acid, alkali, and 6-deoxy-6-perhalogeno-gamma-cyclodextrin as raw materials; and recrystallization can be simply performed on the sugammadex sodium crude product generated by reaction for only one time, and therefore, high purity sugammadex sodium can be obtained. The method has advantages of fast reaction, less impurity generation, simple subsequent purifying and high product purity; and the method is good in economy, low in energy consumption, high in production efficiency, and suitable for commercial process.

Description

technical field [0001] The invention belongs to the field of pharmacy, in particular to a method for synthesizing sugammadex sodium by microwave reaction. Background technique [0002] The chemical name of sugammadex sodium is 6A, 6B, 6C, 6D, 6E, 7F, 6G, 6H-octa-S-(2-carboxyethyl)-6A, 6B, 6C, 6D, 6E, 7F, 6G, 6H-octathio-γ-cyclodextrin, octasodium salt, the structural formula is: [0003] [0004] Sugammadex sodium is a new type of muscle relaxant reversal agent developed by Organon in the Netherlands. It is clinically used to reverse the neuromuscular blockade of rocuronium or vecuronium. It has a good curative effect and has excellent safety; since the European Union approved its listing in July 2008, it has been listed in Japan, South Korea, the United States and other countries, and is being declared for production and listing in my country. [0005] At present, there are few reports on the preparation process of sugammadex sodium at home and abroad, and the basic pur...

Claims

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Application Information

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IPC IPC(8): C08B37/16
CPCC08B37/0012
Inventor 郭辉
Owner HEFEI BOSIKC PHARMTECH CO LTD
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