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Method for purifying clindamycin hydrochloride

A technology of clindamycin hydrochloride alcoholate and clindamycin hydrochloride, which is applied in the field of purification of clindamycin hydrochloride, can solve problems such as environmental hazards and are not mentioned, achieves improved synthesis yield and reduced production cost , the effect of reducing the emulsification effect

Active Publication Date: 2016-09-21
NINGXIA TAIYICIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the chlorination reaction of this process is completed, there is an excessive amount of DMF (N,N-dimethylformamide) reagent, which is easily decomposed into dimethylamine in case of strong alkali, causing environmental hazards
[0005] At present, about reducing emulsification, improving clindamycin alkali extraction yield literature, there are methods such as replacing phosphorus oxychloride with solid phosgene as chlorination reagent method, alkali hydrolysis carries out methods such as alkali extraction with dichloromethane, and utilize macroporous resin The technology of purifying clindamycin hydrochloride has not been mentioned yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 100ml of clindamycin adduct solution (concentration: 200mg / ml), at a speed of 2.0BV / h, control the temperature at 30±2°C, and put it into the macroporous resin column until the feed solution is completely fed. After feeding the feed liquid, wash it with 1,2-dichloroethane until it is colorless, and then elute it with methanol at a rate of 1.5BV / h. The clindamycin adduct peak appears in the HPLC test Finally, collect the clindamycin adduct eluate, when the liquid phase detection clindamycin adduct concentration reaches about 100ug / ml, stop eluting, combine eluate total 298ml (concentration 66mg / ml), receive The rate is 98.34%.

[0030] Add the above eluent to a 500ml three-necked reaction flask, control the temperature at 45±2°C, and distill under reduced pressure until a brownish-yellow oil is precipitated. When no methanol condensate is added to the distillate bottle, stop concentrating to obtain clindamycin adduct Concentrates.

[0031] Add 50ml of butyl acetat...

Embodiment 2

[0036]Take 100ml of clindamycin adduct solution (concentration: 200mg / ml), at a speed of 2.3BV / h, control the temperature at 30±2°C, and put it into the macroporous resin column until the feed solution is completely fed. After feeding the feed liquid, wash it with 1,2-dichloroethane until it is colorless, and then elute it with methanol at a rate of 1.6BV / h. The clindamycin adduct peak appears in the HPLC test Finally, collect the clindamycin adduct eluent, when the liquid phase detection clindamycin adduct concentration reaches about 100ug / ml, stop eluting, combine the total 312ml (concentration 63mg / ml) of eluate, receive The rate is 98.28%.

[0037] Add the above eluent to a 500ml three-necked reaction flask, control the temperature at 45±2°C, and distill under reduced pressure until a brownish-yellow oil is precipitated. When no methanol condensate is added to the distillate bottle, stop concentrating to obtain clindamycin adduct Concentrates.

[0038] Add 50ml of butyl ...

Embodiment 3

[0043] Take 100ml of clindamycin adduct solution (concentration: 200mg / ml), at a speed of 2.5BV / h, control the temperature at 30±2°C, and put it into the macroporous resin column until the feed solution is completely fed. After feeding the feed liquid, wash it with 1,2-dichloroethane until it is colorless, and then elute it with methanol at a rate of 1.7BV / h. The clindamycin adduct peak appears in the HPLC test Finally, collect the clindamycin adduct eluate, when the liquid phase detection clindamycin adduct concentration reaches about 100ug / ml, stop eluting, combine eluate total 318ml (concentration 62mg / ml), receive The rate is 98.58%.

[0044] Add the above eluent to a 500ml three-necked reaction flask, control the temperature at 45±2°C, and distill under reduced pressure until a brownish-yellow oil is precipitated. When no methanol condensate is added to the distillate bottle, stop concentrating to obtain clindamycin adduct Concentrates.

[0045] Add 50ml of butyl acetat...

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Abstract

The invention relates to a method for purifying clindamycin hydrochloride. The process comprises process steps as follows: clindamycin hydrochloride adduct reaction liquid is subjected to macroporous resin adsorption and methyl alcohol desorption; obtained desorbed solution is subjected to reduced pressure distillation and concentration, then is dissolved by butyl acetate solvent, and is subjected to alkaline hydrolysis, alkaline extraction and activated carbon decoloration, and clindamycin alkali decolored solution is obtained; a clindamycin hydrochloride product is obtained after acetone crystallization conversion. According to the method, the macroporous resin is utilized in the clindamycin hydrochloride adduct reaction liquid, so as to facilitate alkaline hydrolysis and alkaline extraction and separation processes, reduce an emulsification effect, improve the clindamycin hydrochloride synthesis yield by more than 6%, reduce a solvent loss, lower production costs, and increase economic benefits; the DMF recovery is facilitated, the cost for raw materials is saved, the influence of DMF on the environment is reduced, and the ecological environment is preserved.

Description

technical field [0001] The invention belongs to the technical field of antibiotic synthesis, in particular to a purification method of clindamycin hydrochloride. Background technique [0002] Clindamycin hydrochloride, also known as clindamycin hydrochloride, the chemical name is 6-(1-methyl-trans-4-propyl-L-2-pyrrolidinecarboxamido)-1-thio -7-Chloro-6,7,8-trideoxy-L-threo-α-D-galactopyranoside hydrochloride, the molecular formula is C 18 h 33 CLN 2 o 5 SHCL is a semi-synthetic derivative of lincomycin hydrochloride, that is, the structure of lincomycin hydrochloride is modified, and the hydroxyl on the C7 position of lincomycin hydrochloride is replaced by a chlorine atom. [0003] Clindamycin hydrochloride is a safe and effective broad-spectrum antibacterial drug, the antibacterial activity is 4 to 8 times that of lincomycin hydrochloride, and the adverse reactions are low. Clinically, it is mainly used for osteomyelitis, infection caused by anaerobic bacteria, respir...

Claims

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Application Information

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IPC IPC(8): C07H15/16C07H1/06
CPCC07H1/06C07H15/16
Inventor 裴立忠王勇平张鹏张江飞
Owner NINGXIA TAIYICIN BIOTECH CO LTD
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