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Production process of green and nontoxic sulfobutyl ether-beta-cyclodextrin sodium salt

A technology of sulfobutyl ether and cyclodextrin sodium is applied in the production process field of green non-toxic sulfobutyl ether-β-cyclodextrin sodium salt, which can solve the problem of difficulty in industrial production, low product yield and safety. problems such as low coefficient, to achieve the effect of high production efficiency, high product yield and low production cost

Pending Publication Date: 2022-01-18
秦大伟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to overcome the above-mentioned defects of the prior art, the embodiments of the present invention provide a production process of green nontoxic sulfobutyl ether-β-cyclodextrin sodium salt. The technical problems to be solved by the present invention are: low synthesis yield, low safety factor Problems such as low production efficiency and complex process make the product yield not high and it is difficult to meet the needs of industrial production

Method used

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  • Production process of green and nontoxic sulfobutyl ether-beta-cyclodextrin sodium salt

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Embodiment 1

[0029] like figure 1 As shown, the embodiment is as follows: the present invention provides a production process of green non-toxic sulfobutyl ether-β-cyclodextrin sodium salt, comprising the following steps:

[0030] S1: provide 80kg tetrahydrofuran, 77kg acetyl chloride, 50mg zinc chloride, 300kg sodium sulfite aqueous solution, 5g β-cyclodextrin, 10ml 200g / L sodium hydroxide aqueous solution;

[0031] S2: Preparation of monomeric 4-chloro-butanesulfonic acid:

[0032] Pour 80kg of tetrahydrofuran and 77kg of acetyl chloride into the container, and add 50mg of zinc chloride, then react under the catalysis of 50mg of zinc chloride to first obtain an intermediate product, then the intermediate product is fully reacted in 300kg of sodium sulfite aqueous solution, and then through Hydrochloric acid hydrolysis to obtain 4-chloro-butanesulfonic acid;

[0033] S3: Synthesis reaction: Synthesis of sulfobutyl ether-β-cyclodextrin sodium salt:

[0034] Weigh 5g of β-cyclodextrin an...

Embodiment 2

[0038] like figure 1 As shown, the embodiment is as follows: the present invention provides a production process of green non-toxic sulfobutyl ether-β-cyclodextrin sodium salt, comprising the following steps:

[0039] S1: Provide 80kg tetrahydrofuran, 70kg acetyl chloride, 45mg zinc chloride, 300kg sodium sulfite aqueous solution, 5g β-cyclodextrin, 10ml 200g / L sodium hydroxide aqueous solution;

[0040] S2: Preparation of monomeric 4-chloro-butanesulfonic acid:

[0041] Pour 80kg of tetrahydrofuran and 77kg of acetyl chloride into the container, and add 50mg of zinc chloride, then react under the catalysis of 50mg of zinc chloride to first obtain an intermediate product, then the intermediate product is fully reacted in 300kg of sodium sulfite aqueous solution, and then through Hydrochloric acid hydrolysis to obtain 4-chloro-butanesulfonic acid;

[0042] S3: Synthesis reaction: Synthesis of sulfobutyl ether-β-cyclodextrin sodium salt:

[0043] Weigh 5g of β-cyclodextrin an...

Embodiment 3

[0047] like figure 1 As shown, the embodiment is as follows: the present invention provides a production process of green non-toxic sulfobutyl ether-β-cyclodextrin sodium salt, comprising the following steps:

[0048] S1: provide 80kg tetrahydrofuran, 65kg acetyl chloride, 40mg zinc chloride, 300kg sodium sulfite aqueous solution, 5g β-cyclodextrin, 10ml 200g / L sodium hydroxide aqueous solution;

[0049] S2: Preparation of monomeric 4-chloro-butanesulfonic acid:

[0050] Pour 80kg of tetrahydrofuran and 77kg of acetyl chloride into the container, and add 50mg of zinc chloride, then react under the catalysis of 50mg of zinc chloride to first obtain an intermediate product, then the intermediate product is fully reacted in 300kg of sodium sulfite aqueous solution, and then through Hydrochloric acid hydrolysis to obtain 4-chloro-butanesulfonic acid;

[0051] S3: Synthesis reaction: Synthesis of sulfobutyl ether-β-cyclodextrin sodium salt:

[0052] Weigh 5g of β-cyclodextrin an...

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Abstract

The invention discloses a production process of green and nontoxic sulfobutyl ether-beta-cyclodextrin sodium salt, and particularly relates to the field of sulfobutyl ether-beta-cyclodextrin sodium salt. The process comprises the following steps: S1: providing tetrahydrofuran, acetyl chloride, zinc chloride, a sodium sulfite aqueous solution, beta-cyclodextrin and a sodium hydroxide aqueous solution; S2: preparation of a monomer 4-chloro-butanesulfonic acid: pouring tetrahydrofuran and acetyl chloride into a container, adding zinc chloride to prepare an intermediate product, introducing the intermediate product into a sodium sulfite aqueous solution for full reaction, and carrying out hydrolyzing with hydrochloric acid to obtain the 4-chloro-butanesulfonic acid. According to the invention, tetrahydrofuran and acetyl chloride react to obtain 4-chlorine-butanesulfonic acid, then beta-cyclodextrin and 4-chlorine-butanesulfonic acid serve as raw materials and are added into a container to react, and compared with the method that 1, 4-butanesultone with toxicity serves as a preparation raw material, the process is more environmentally friendly and free of toxicity, and improves certain safety.

Description

technical field [0001] The invention relates to the field of sulfobutyl ether-β-cyclodextrin sodium salt, and more particularly, the invention relates to a production process of green nontoxic sulfobutyl ether-β-cyclodextrin sodium salt. Background technique [0002] Sulfobutyl ether-β-cyclodextrin sodium is a new type of anionic high water-soluble cyclodextrin derivative, which can be well included with drug molecules to form non-covalent complexes, thereby improving the stability and water-solubility of drugs. , safety, reduce nephrotoxicity, ease drug hemolysis, control drug release rate, mask bad odor, etc. Compared with β-cyclodextrin, it has better water solubility, less hemolysis and low nephrotoxicity, and is a new type of pharmaceutical excipient with very broad application prospects; [0003] Relevant patent one: CN103694376B, it adopts two steps, namely synthesis reaction: temperature control 20-30 ℃, add organic solvent and the sodium hydroxide aqueous solution ...

Claims

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Application Information

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IPC IPC(8): C08B37/16
CPCC08B37/0012
Inventor 秦大伟王利振秦硕卿
Owner 秦大伟
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