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Method for preparing sulfobutyl ether-beta-cyclodextrin by adopting pipeline reactor

The technology of a pipeline reactor and sulfobutyl ether, which is applied in the field of pharmaceutical excipients, can solve the problems of high requirements on the reaction rate and efficiency of the pipeline reactor, long pipeline and difficult realization, etc., and achieves flexible reaction, improved catalytic activity, and improved conversion. rate effect

Pending Publication Date: 2022-04-19
贵州省欣紫鸿药用辅料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main reason is that the pipeline reactor has high requirements on the reaction rate and efficiency. When the reaction rate is very low, the required pipeline is too long, which is difficult to realize in industry.

Method used

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  • Method for preparing sulfobutyl ether-beta-cyclodextrin by adopting pipeline reactor
  • Method for preparing sulfobutyl ether-beta-cyclodextrin by adopting pipeline reactor
  • Method for preparing sulfobutyl ether-beta-cyclodextrin by adopting pipeline reactor

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Experimental program
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Effect test

Embodiment 1

[0046] A method for preparing sulfobutyl ether-β-cyclodextrin (SBE1-β-CD) with a degree of substitution of 1 in this embodiment, the specific preparation process is as follows:

[0047] (1) Add 20 ml of purified water to the reaction flask at room temperature, add 0.84 gram of sodium hydroxide during stirring, then add 20 grams of β-cyclodextrin, filter after all the β-cyclodextrin dissolves, remove insoluble matter, A solution of β-cyclodextrin is obtained.

[0048](2) Set the temperature of the pipeline reactor to 70-80°C, turn on the β-cyclodextrin solution delivery pump, and set the speed at 140rpm; after 5 minutes, turn on the 1,4-butane sultone dosing pump, and set the speed 20rpm; at the same time, turn on the sodium hydroxide solution delivery pump and set the speed at 10rpm. The ratio of the amount of substances controlling the mixed reaction of β-cyclodextrin and 1,4-butane sultone is 1:1.2.

[0049] (3) After 15 minutes of reaction in the pipeline reactor, turn on...

Embodiment 2

[0052] A method for preparing sulfobutyl ether-β-cyclodextrin (SBE4-β-CD) with a degree of substitution of 4 in this embodiment, the specific preparation process is as follows:

[0053] (1) Add 20 ml of purified water to the reaction flask at room temperature, add 3.5 grams of sodium hydroxide during stirring, then add 20 grams of β-cyclodextrin, filter after all the β-cyclodextrin dissolves, and remove insoluble matter, A solution of β-cyclodextrin is obtained.

[0054] (2) Set the temperature of the pipeline reactor to 70-80°C, turn on the β-cyclodextrin solution delivery pump, and set the speed at 72rpm; after 5 minutes, turn on the 1,4-butane sultone dosing pump, a total of 4 The channel is dripped with 1,4-butane sultone, and the pipeline of each channel is extended by 1.5 meters in turn, and the set speed is 72rpm; at the same time, the sodium hydroxide solution delivery pump is turned on, and the set speed is 40rpm. The ratio of the amount of substances controlling the...

Embodiment 3

[0058] A method for preparing sulfobutyl ether-β-cyclodextrin (SBE1-β-CD) with a degree of substitution of 7 in this embodiment, the specific preparation process is as follows:

[0059] (1) Add 20 ml of purified water to the reaction flask at room temperature, add 7.4 grams of sodium hydroxide during stirring, then add 20 grams of β-cyclodextrin, filter after all the β-cyclodextrin dissolves, and remove insoluble matter, A solution of β-cyclodextrin is obtained.

[0060] (2) Set the temperature of the pipeline reactor at 70-80°C, turn on the β-cyclodextrin solution delivery pump, and set the speed at 72rpm; after 5 minutes, turn on the 1,4-butane sultone dosing pump, a total of 7 The channel is dripped with 1,4-butane sultone, and the pipeline of each channel is extended by 1.5 meters in turn, and the set speed is 72rpm; at the same time, the sodium hydroxide solution delivery pump is turned on, and the set speed is 70rpm. The ratio of the amount of substances controlling the...

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Abstract

The invention belongs to the technical field of pharmaceutical excipients, and discloses a method for preparing sulfobutyl ether-beta-cyclodextrin by adopting a pipeline reactor. The preparation method comprises the following steps: adding beta-cyclodextrin into a sodium hydroxide aqueous solution, stirring until the beta-cyclodextrin is completely dissolved, filtering, and removing insoluble substances to obtain a beta-cyclodextrin solution; the obtained beta-cyclodextrin solution is conveyed to a pipeline reactor through a conveying pump, the temperature of the pipeline reactor is set to be 70-80 DEG C, and then a 1, 4-butanesultone conveying pump and an alkaline catalytic solution conveying pump are started step by step for a reaction; and after the reaction is completed, starting an acid liquor delivery pump for neutralization, and then filtering and drying to obtain the sulfobutyl ether-beta-cyclodextrin. The preparation method has the advantages that the reaction is easy to control, the operation is simple, and continuous production can be realized.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical auxiliary materials, and in particular relates to a method for preparing sulfobutyl ether-β-cyclodextrin by using a pipeline reactor. Background technique [0002] Cyclodextrin (CD for short) is a cyclic oligosaccharide of D-glucose, which is isolated from the reaction of starch cyclodextrin carbonyl conversion enzyme, and β-glucopyranose with chair conformation passes through α-(1,4) It is connected by glycosidic bonds and has a special non-polar tire-like ring structure. Its chemical structure is as follows: [0003] [0004] Natural cyclodextrin includes n=4, also known as α-CD; n=5, β-CD; n=6, γ-CD three conformations. In the field of pharmaceutical preparations, cyclodextrin and its derivatives can encapsulate various organic and inorganic guest molecules. Alkylated, hydroxyalkylated, sulfoalkylated, and sulfonated-β-cyclodextrin derivatives have been developed in order to change ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16
CPCC08B37/0012
Inventor 宋波沈惠
Owner 贵州省欣紫鸿药用辅料有限公司
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