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A kind of method for preparing high-purity Calcium Calcobutrol

A high-purity technology for calcobutrol calcium, which is applied in the field of preparing high-purity calcobutrol calcium, can solve the problems of being unfavorable for scale-up production, unfriendly to the environment, and high operating costs, and achieves improved stability, bioavailability, and environmental friendliness. , the effect of improving the purity

Active Publication Date: 2021-03-05
CHEN STONE GUANGZHOU CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This operation cost is high, the operation is cumbersome, it is not conducive to large-scale production, and a large amount of resin and ammonia water are used, which is very unfriendly to the environment

Method used

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  • A kind of method for preparing high-purity Calcium Calcobutrol
  • A kind of method for preparing high-purity Calcium Calcobutrol
  • A kind of method for preparing high-purity Calcium Calcobutrol

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Embodiment Construction

[0044] The method for preparing high-purity Calcium Cobutrol is described in detail below by way of examples.

[0045] The first step, neutralization reaction

[0046] At 10-30°C, add 2Kg of water and 1Kg of butanol (Formula 2) into the reaction kettle, stir to dissolve, then add 300g of sodium hydroxide, the pH of the system is measured to be greater than 14, heat to reflux for 1 hour, and drop in 25Kg of ethanol , kept under reflux for 1 hour, cooled and aged, the water content was 6%, filtered, the filter cake was washed with an appropriate amount of absolute ethanol or 95% ethanol, and dried to obtain 1.05 Kg of butanol sodium salt of formula 3.

[0047] Compound of formula 3 1 H-NMR such as figure 1 shown. Compound of formula 3 13 C-NMR such as figure 2 shown.

[0048] 1 H-NMR (MeOD): δ1.50-2.40(m), 2.50-3.50(m), 3.50-4.00(m).

[0049] 13 C-NMR (MeOD): δ 45.86, 47.1-48.1 (m), 58.65, 58.71, 59.34, 60.16, 63.83, 70.14, 178.09, 178.24, 178.40.

[0050] The second ...

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Abstract

The invention discloses a method for preparing high-purity kobutrol calcium, which comprises: (1) using butanol as a starting material to prepare an alkali metal salt of butanol; (2) reacting the alkali metal salt of butanol with a calcium source Get Cobutrol Calcium. The present invention also provides a crystal form of Calcobutrol, represented by 2θ angles in the X-ray powder diffraction diagram, at 8.448°, 8.970°, 9.329°, 9.711°, 11.428°, 12.309°, 13.744°, There are characteristic diffraction peaks at 14.443°, 15.715°, and 16.953°. The preparation method of the present invention can obtain high-purity kobutrol calcium.

Description

technical field [0001] The application relates to a method for preparing high-purity Calcium Cobutrol. Background technique [0002] In the field of gadolinium-containing contrast agents, gadobutrol is sold commercially around the world under the trade names Gadavist or Gadavist. Gadobutrol is a non-ionic coordination compound composed of gadolinium and a macrocyclic ligand dihydroxy-hydroxy-methyl-propyl-tetraazacyclododecane-triacetic acid (butrol). The gadolinium-containing contrast agent is approved for contrast-enhanced magnetic resonance imaging (CE-MRI) diagnosis of multiple parts of the human body, including the brain, spinal cord, blood vessels, liver and kidneys. Gadobutrol contains a high concentration of ionic T1-relaxers, which contribute to its excellent image quality. [0003] It is known that in most gadolinium-containing contrast agent preparations (including gadobutrol), calcium complexes are used as additives, and excess calcium complex forms the ligand ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/02
CPCC07B2200/13C07D257/02
Inventor 周磊谭俊荣赖英杰梁龙杨永年
Owner CHEN STONE GUANGZHOU CO LTD
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