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Method for reducing dehydrolincomycin in lincomycin hydrochloride

A technology of lincomycin hydrochloride and hydrogen lincomycin, which is applied in the field of medicine, can solve the problems of high industrialization cost, expensive palladium carbon, high reaction pressure, etc., to reduce the waste water treatment process, improve the safety production factor, and be easy to recycle Effect

Inactive Publication Date: 2018-08-17
XINYU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, palladium carbon is expensive, the cost of industrialization is high, and the solvent is used in the reaction, and the reaction pressure is high, so there is a certain risk

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The invention provides a method for reducing dehydrolincomycin in lincomycin hydrochloride, comprising the following steps:

[0018] S1, dissolving 100g of lincomycin hydrochloride in 200mL of purified water to obtain an aqueous solution;

[0019] S2, adding 10g of Raney nickel catalyst to the aqueous solution of step S1;

[0020] S3, introducing hydrogen gas into the aqueous solution in step S2, stirring and reacting for 6 hours, the pressure in the reaction process is ≤0.02Mpa, and the reaction solution is obtained;

[0021] S4, filter the reaction solution, filter out the Raney nickel catalyst, and obtain the filtrate;

[0022] S5, washing away the reaction solution attached to the surface of the Raney nickel catalyst with 600mL purified water to obtain the washing solution;

[0023] S6. Combine the filtrate and the washing liquid, and obtain lincomycin hydrochloride after crystallization.

[0024] In this embodiment, the removal rate of dehydrolincomycin is 90%, ...

Embodiment 2

[0026] The invention provides a method for reducing dehydrolincomycin in lincomycin hydrochloride, comprising the following steps:

[0027] S1, dissolving 100g of lincomycin hydrochloride in 300mL of purified water to obtain an aqueous solution;

[0028] S2. Add the Raney nickel catalyst used in Example 1 to the aqueous solution in step S1;

[0029] S3. Pass hydrogen into the aqueous solution in step S2, stir and react for 8 hours, and the pressure in the reaction process is ≤0.02Mpa to obtain a reaction solution;

[0030] S4, filter the reaction solution, filter out the Raney nickel catalyst, and obtain the filtrate;

[0031] S5, washing away the reaction solution attached to the surface of the Raney nickel catalyst with 600mL purified water to obtain the washing solution;

[0032] S6. Combine the filtrate and the washing liquid, and obtain lincomycin hydrochloride after crystallization.

[0033] In this embodiment, the removal rate of dehydrolincomycin is 88%, and the yie...

Embodiment 3

[0035] The invention provides a method for reducing dehydrolincomycin in lincomycin hydrochloride, comprising the following steps:

[0036] S1, dissolving 50g of lincomycin hydrochloride in 200mL of purified water to obtain an aqueous solution;

[0037] S2. Add 5 g of the Raney nickel catalyst used in Example 2 to the aqueous solution of step S1;

[0038] S3, introducing hydrogen gas into the aqueous solution in step S2, stirring and reacting for 7 hours, the pressure in the reaction process is ≤0.02Mpa, and the reaction solution is obtained;

[0039] S4, filter the reaction solution, filter out the Raney nickel catalyst, and obtain the filtrate;

[0040] S5, washing away the reaction solution attached to the surface of the Raney nickel catalyst with 300mL purified water to obtain a washing solution;

[0041] S6. Combine the filtrate and the washing liquid, and obtain lincomycin hydrochloride after crystallization.

[0042] In this embodiment, the removal rate of dehydrolin...

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PUM

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Abstract

The invention discloses a method for reducing dehydrolincomycin in lincomycin hydrochloride, and the method comprises the following steps: S1, dissolving lincomycin hydrochloride in purified water with the weight of 2 to 4 times of the weight of the lincomycin hydrochloride to obtain an aqueous solution; S2, adding a Raney nickel catalyst with the weight of 1 / 10 of the weight of the lincomycin hydrochloride to the aqueous solution of the step S1; S3, introducing hydrogen into the aqueous solution of the step S2 for reaction for 6-8h to obtain a reaction liquid; S4, filtering the reaction liquid to filter out the Raney nickel catalyst to obtain a filtrate; S5, using purified water to wash the reaction liquid attached to the surface of the Raney nickel catalyst away to obtain a washing liquid; and S6, combining the filtrate and the washing liquid, and crystallizing to obtain the lincomycin hydrochloride; the method adopts the Raney nickel catalyst for hydrogenation reaction, the cost issuccessfully reduced, and the method is suitable for industrial production; the hydrogenation reaction is carried out under normal pressure, and the safety production coefficient is improved.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for reducing dehydrolincomycin in lincomycin hydrochloride. Background technique [0002] Lincomycin hydrochloride is a narrow-spectrum antibiotic, which has a good effect on Gram-positive cocci, especially anaerobic bacteria, Staphylococcus aureus and pneumococcus. Its mechanism of action is a bacteriostatic agent, mainly inhibiting the synthesis of bacterial cell proteins Clinically, it is mainly used for various infections caused by sensitive bacteria, such as pneumonia, meningitis, endocarditis, cellulitis, tonsillitis, erysipelas, boils and urinary system infections. Because this product can enter bone tissue and has a special affinity with bone, it is especially suitable for infections caused by anaerobic bacteria and staphylococcus aureus osteomyelitis. [0003] Lincomycin hydrochloride mainly contains impurities dehydrolincomycin, α-amide isomers, and lincomyci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/16C07H1/06C07H1/00
CPCC07H1/00C07H1/06C07H15/16
Inventor 许计强王珍丁振东
Owner XINYU PHARM CO LTD
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