Preparation methods of sulbenicillin sodium and injection thereof

A technology of sulfobenicillin sodium and solution is applied in the field of preparation of sulfobenicillin sodium and its injection, and can solve the problems of many by-products, complicated reactions, waste of raw materials, etc., and achieve simple steps, high product purity, and few reaction impurities. Effect

Inactive Publication Date: 2010-08-18
HUNAN ERKANG XIANGYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, in the preparation process of sulbenicillin sodium, the reaction is com

Method used

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  • Preparation methods of sulbenicillin sodium and injection thereof
  • Preparation methods of sulbenicillin sodium and injection thereof
  • Preparation methods of sulbenicillin sodium and injection thereof

Examples

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Example Embodiment

[0024] Combine figure 1 In a typical embodiment of the preparation method of sulfbenicillin sodium of the present invention, the method includes the following steps:

[0025] Sulfonation: Mix dichloroethane and dioxane with stirring, lower the temperature to 0-5°C, introduce sulfur trioxide, add phenylacetic acid, and raise the temperature to 30-45°C and stir to obtain solution A.

[0026] Dioxane will form a complex with sulfur trioxide. Therefore, delaying the addition time of sulfur trioxide will reduce the consumption of dioxane and sulfur trioxide; and the low temperature of 0~5℃ will reduce the reaction rate. Save raw materials.

[0027] The reaction equation of the above-mentioned dioxane and sulfur trioxide reaction to form dioxane sulfonate is as follows:

[0028]

[0029] Hydrolysis: Pour the above solution A into an appropriate amount of purified water at a temperature of 18-22°C, cool to below 10°C, stir and let stand to separate into an upper aqueous layer and a lower or...

Example Embodiment

[0087] Example

[0088] During the preparation of Sulbenicillin Sodium, all the raw materials used are shown in Table 1.

[0089] Table 1 The raw materials used in the preparation process of Sulbenicillin Sodium and the amount used.

[0090] Accessory name

[0091] The preparation method is as follows:

[0092] Vulcanization: add the prescription amount of industrial grade dichloroethane and industrial grade dioxane to the sulfonation tank, turn on the stirring, open the chilled water valve of the sulfonation tank jacket, cool down to below 5°C, turn on the sulfur trioxide Intake valve. When sulfur trioxide is introduced for sulfonation, control the sulfur trioxide flow rate, keep the temperature of the sulfonation tank not exceeding 10°C, and check the weight of the sulfur trioxide generating tank at any time, calculate by weight reduction method, and add the prescription amount of industrial grade three After oxidizing the sulfur, close the valve of the sulfur trioxide cylinder...

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Abstract

The invention discloses a preparation method of sulbenicillin sodium, which comprises the following steps of: sulfonating, hydrolyzing, crystallizing, ion-exchanging, acidylating, condensing, extracting and salifying to obtain sulbenicillin sodium. The method has the advantages of simple technological steps, fewer reaction impurities and high product purity, and the yield is higher than 50%. Meanwhile, the invention also relates to a preparation method of a sulbenicillin sodium injection.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a preparation method of sulfbenicillin sodium and its injection. Background technique [0002] Sulbenicillin Sodium, also known as Sulbenicillin Sodium, Sulbenicillin Sodium, Gedacillin; generally white or light yellow powder; odorless, mild taste; hygroscopic; easily soluble in water, easily soluble in methanol , Slightly soluble in ethanol, very slightly soluble in absolute ethanol, insoluble in acetone, chloroform or benzene. [0003] Sulbenicillin sodium is a semi-synthetic anti-pseudomonal penicillin. Its antibacterial spectrum is similar to carbenicillin, and its antibacterial effect is strong. It plays a bactericidal effect by inhibiting the synthesis of bacterial cell walls; Enterobacteriaceae such as Bacillus, Citrobacter, Salmonella, and Shigella, and other Gram-negative bacteria such as Pseudomonas aeruginosa, Haemophilus influenzae, and Neisseria have antibacterial effects; ...

Claims

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Application Information

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IPC IPC(8): C07D499/62C07D499/16A61K9/08A61K31/43A61P31/04
Inventor 帅放文王向峰章家伟杨海明
Owner HUNAN ERKANG XIANGYAO PHARMA
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