Method for efficiently preparing low-calcium-content folinic acid

A technology of calcium content and folinic acid, applied in the direction of organic chemistry, etc., can solve problems such as no reported preparation, low folinic acid and the like

Inactive Publication Date: 2015-01-14
SHANGHAI HUILUN BIOLOGICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Existing published method also does not report the me

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation of embodiment 1 folinic acid

[0022] Add 27L of water into a 50L glass reactor, lower the temperature to below 10°C, add the prepared calcium folinate aqueous solution (900g dissolved in 13.5L of water) and 1.2N hydrochloric acid dropwise into the reactor at the same time, and maintain the pH of the system at 2.7-2.9 , the temperature is 6°C to 10°C, and the dropwise addition is completed in 3.5 hours. Centrifuge and rinse with water (4L) to obtain a wet product.

[0023] Add 9L of deionized water into a 20L glass reactor, cool down to 6°C-10°C, add the above wet product to wash, centrifugal filter, rinse with water (4L), and dry the wet product through fluidized bed for 1 hour before 40°C Vacuum drying for 24 hours yielded 686 g of light yellow powder with a water content of 8.1%. The calcium content tested by atomic absorption method is 0.006%, and the residue on ignition is 0.04%.

Embodiment 2

[0024] The preparation of embodiment 2 folinic acid

[0025] Add 300mL water into a 1L four-necked bottle, cool down to below 6°C, add the prepared calcium folinate aqueous solution (20g dissolved in 600mL water) and 2.4N hydrochloric acid to the reaction flask at the same time, to maintain the pH value of the system at 2.3-2.5, The temperature is 2°C-6°C, and the dropwise addition is completed in 3 hours. Filter and wash the filter cake with water to obtain a wet product. The wet product was beaten at room temperature, rinsed, and vacuum-dried at 20°C for 48 hours to obtain 15.5 g of yellow powder with a water content of 8.8%. The calcium content tested by atomic absorption method is 0.004%, and the residue on ignition is 0.03%.

Embodiment 3

[0026] The preparation of embodiment 3 folinic acid

[0027] Add 700mL water into a 1L four-necked bottle, cool down to below 12°C, add the prepared calcium folinate aqueous solution (20g dissolved in 120mL water) and 0.3N hydrochloric acid to the reaction flask at the same time, to maintain the pH of the system at 3.1-3.3, The temperature is 8°C to 12°C, and the dropwise addition is completed in 2.5 hours. Filter and wash the filter cake with water to obtain a wet product. The wet product was beaten at room temperature, rinsed, and vacuum-dried at 40°C for 24 hours to obtain 14.8 g of light yellow powder with a water content of 7.8%. The atomic absorption method tested the calcium content to be 0.022%, and the ignition residue was 0.09%.

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Abstract

The invention relates to a method for efficiently preparing low-calcium-content folinic acid. The method for efficiently preparing the low-calcium-content folinic acid comprises the following steps: dropwise adding a dissolved folinic acid aqueous solution and diluted hydrochloric acid with certain concentration into water, strictly controlling system temperature and pH value, separating out solids, washing, and drying, so that the low-calcium-content folinic acid is obtained. The obtained low-calcium-content folinic acid product is good in solid physical property and low in calcium content, and operation is easy, so that the method for efficiently preparing the low-calcium-content folinic acid is applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis medicine preparation and relates to a method for efficiently preparing folinic acid with low calcium content. Background technique [0002] Leucovorin, chemical name N-[4-[(2-amino-5-formyl-1,4,5,6,7,8-hexahydro-4-oxo-6-pteridinyl) Methyl]amino]benzoyl-L-glutamic acid has been widely used in combination chemotherapy for cancer. [0003] When folinic acid is used as a medicine, it is mostly used in the form of calcium salt. However, when a large dose is required clinically (200-500mg / m 2 / d), sodium folinate, which is more soluble in water, is better than calcium folinate. When it is compatible with other drugs or infusions, sodium folinate has better compatibility, and there is no need to worry about ion metabolism caused by excessive calcium ions entering the body disorder. [0004] Since the raw materials of sodium folinate prepared by the existing disclosed technology all have cr...

Claims

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Application Information

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IPC IPC(8): C07D475/04
CPCC07D475/04
Inventor 李文华秦继红
Owner SHANGHAI HUILUN BIOLOGICAL TECH CO LTD
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