Preparation method of ciprofloxacin lactate

A technology of ciprofloxacin lactate and ciprofloxacin, which is applied in the direction of organic chemistry, can solve the problems of prolonging the production cost of the process flow, and achieve the effects of shortening the production cycle, simplifying the process flow, and low impurity content

Active Publication Date: 2017-05-10
HENAN KANGDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Ciprofloxacin lactate is produced by neutralizing ciprofloxacin hydrochloride with alkali to form ciprofloxacin, and then the salt-forming reaction between ciprofloxacin and a salt-forming agent, in which there are two steps of neutralization reaction and salt-forming reaction The operation is dir

Method used

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  • Preparation method of ciprofloxacin lactate

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Embodiment 1

[0031] A preparation method of ciprofloxacin lactate, comprising the following steps:

[0032] 1) Put 10g of ciprofloxacin hydrochloride and 100g of purified water into the flask, raise the temperature to 53°C, and stir to dissolve;

[0033] 2) Under the condition of 55°C, add about 0.19g of ammonia water with a concentration of 7wt% to the solution obtained in step 1), crystals will be precipitated in the solution, and the crystals will be grown for 25 minutes; then continue to drop ammonia water to the pH of the solution 6.8, after cooling the solution to 30°C, grow the crystal for 4 hours; control the dripping speed of ammonia water so that the ammonia solution is added dropwise for 30 minutes until the pH value of the solution reaches the requirement;

[0034] 3) The crystals obtained in step 2) were collected by filtration, washed three times with 50g of purified water, and then washed twice with 20g of ethanol with a volume concentration of 95%, and then vacuumed the cry...

Embodiment 2

[0039] A preparation method of ciprofloxacin lactate, comprising the following steps:

[0040] 1) Put 10g of ciprofloxacin hydrochloride and 100g of purified water into the flask, raise the temperature to 55°C, and stir to dissolve;

[0041] 2) Under the condition of 55°C, add sodium hydroxide solution with a concentration of 4wt% to the solution obtained in step 1) dropwise. When crystals are precipitated in the solution, grow the crystal for 30 minutes; then continue to add sodium hydroxide solution dropwise to The pH in the solution is 7.0. After cooling the solution to 25°C, grow the crystal for 4 hours; control the dropping rate of the sodium hydroxide solution so that the sodium hydroxide solution is added dropwise for 30 minutes until the pH of the solution reaches the requirement;

[0042] 3) The crystals obtained in step 2) were collected by filtration, washed three times with 50g purified water, and then washed twice with 20g ethanol with a volume concentration of 95...

Embodiment 3

[0046] A preparation method of ciprofloxacin lactate, comprising the following steps:

[0047] 1) Put 10g of ciprofloxacin hydrochloride and 120g of purified water into the flask, raise the temperature to 90°C, and stir to dissolve;

[0048] 2) Lower the temperature of the solution obtained in step 1) to 55°C, add dropwise ammonia water with a concentration of 7wt% until crystals are precipitated in the solution, and grow the crystal for 30 minutes; then continue to drop ammonia water until the pH of the solution is 7.0. After cooling down to 30°C, grow the crystal for 4 hours; control the dripping rate of ammonia water so that the ammonia water is added dropwise for 30 minutes until the pH value of the solution reaches the requirement;

[0049] 3) The crystals obtained in step 2) were collected by filtration, washed three times with 50g of purified water, and then washed twice with 20g of ethanol with a volume concentration of 95%, and then vacuumed the crystals at 60°C and a...

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Abstract

The invention belongs to the technical field of medicine preparation and particularly relates to a preparation method of ciprofloxacin lactate. The method comprises the steps as follows: mixing ciprofloxacin hydrochloride with a solvent, adjusting pH with alkali, and performing cooling crystallization, filtration, drying and other steps to obtain ciprofloxacin; mixing ciprofloxacin with the solvent, adding a salt forming agent for a salt forming reaction, and then performing cooling crystallization, filtration, drying and other steps to obtain a finished product of ciprofloxacin lactate. The preparation method is simple to operate, the involved reaction condition is mild and easy to control, ciprofloxacin lactate is prepared in two steps, the refining process is omitted, the production cycle is shortened, the cost is greatly reduced, and the mass yield of ciprofloxacin lactate reaches 95% or higher, and the product purity can reach 99.5%.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and in particular relates to a preparation method of ciprofloxacin lactate. Background technique [0002] Ciprofloxacin lactate, molecular formula C 17 h 18 FN 3 o 3 ·C 3 h 6 o 3 , molecular weight 421.43, chemical name is 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7(1-piperazinyl)-3-quinoline carboxylic acid lactate, its structural formula As shown in the following structure: [0003] , Ciprofloxacin lactate is a non-sterile raw material drug, which is off-white or slightly yellow crystalline powder; odorless, bitter, hygroscopic, CAS number: 97867-33-9. [0004] Ciprofloxacin Lactate is a quinolone drug with broad-spectrum antibacterial effect. It acts on the A subunit of bacterial DNA helicase to inhibit DNA synthesis and replication, leading to bacterial death. Its antibacterial activity is the strongest among the fluoroquinolones widely used at present. It is characteri...

Claims

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Application Information

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IPC IPC(8): C07D215/56
CPCC07D215/56
Inventor 安丽平李红德曹文英李文杰刘红坤孙津鸽孟源
Owner HENAN KANGDA PHARMA
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