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A kind of preparation method of high-yield gadobutrol

A technology of gadobutrol and its compound, which is applied in the field of preparation of high-yield gadobutrol, can solve problems such as the instability of rotenin, prolonged production time, and difficulty in controlling impurities, so as to facilitate scale-up production and reduce production costs , the effect of high purity

Active Publication Date: 2020-08-04
CHEN STONE GUANGZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of DMF acetal-protected fenneline is extremely unstable, it is easy to hydrolyze, and it is difficult to control impurities; when lithium hydroxide is used for hydrolysis, a large amount of water needs to be concentrated, which increases energy consumption and prolongs production time; alkylation The chloroacetic acid used in the step is a highly toxic compound with high risk

Method used

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  • A kind of preparation method of high-yield gadobutrol
  • A kind of preparation method of high-yield gadobutrol
  • A kind of preparation method of high-yield gadobutrol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] The synthesis of embodiment 1 gadobutrol

[0080] The first step: the synthesis of compound 2

[0081]

[0082] (1) Reaction in potassium carbonate solution

[0083] 40L of water was added under stirring, 28.1kg of potassium carbonate and 40L of THF were added, 11.6kg of tertogenin monoformaldehyde 1 was added, and 37.5kg of tert-butyl bromoacetate was added dropwise at 50°C. After the reaction was completed, the organic phase was separated and concentrated to obtain 28.4kg of compound 2, which was directly put into the next reaction.

[0084] (2) Alternatively, react in sodium carbonate solution

[0085] 50 mL of water was added under stirring, 35.0 g of sodium carbonate and 50 mL of THF were added, 20.0 g of rhododendronin monoformaldehyde 1 was added, and 64.7 g of tert-butyl bromoacetate was added dropwise at 50°C. After the reaction was completed, the organic phase was separated and concentrated to obtain 47.3 g of compound 2.

[0086] Compound 2: 1 HNMR (4...

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Abstract

The invention provides a preparation method of high field gadobutrol. Cycleanine monoformaldehyde is used as a raw material, alkylation reaction is carried out with tert-butyl bromoacetate, then the alkylation product is hydrolyzed, and tricarboxylate intermediate is obtained; the tricarboxylate intermediate and 4,4-dimethyl-3,5,8-three oxygen bicyclo [5.1.0] octane react, then complex reaction ofthe reaction product and gadolinium oxide is carried out, and gadobutrol with higher purity and good yield is obtained.

Description

technical field [0001] The invention relates to a preparation method of gadobutrol with high yield. Background technique [0002] Magnetic resonance imaging (MRI) technology has a wide range of applications in the biological and medical fields, and has become a commonly used medical diagnostic method. At present, an important research direction of MRI contrast agents in the world is to develop contrast agents with organ and tissue targeting, so that the contrast agents can be enriched in specific organs and tissues, thereby improving the contrast effect. Gadobutrol It is a new type of powerful magnetic resonance imaging contrast agent approved for contrast-enhanced magnetic resonance imaging (CE-MRI) diagnosis of multiple parts of the human body, including brain, spinal cord, blood vessels, liver and kidney. In addition, gadobutrol contains a high concentration of ionic T1-relaxation potency, and due to its high concentration and high relaxation potency, it shows the high...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/02
CPCC07D257/02
Inventor 赖英杰梁龙龙翔天周磊白礼斌曹本文谭俊荣谢德逊
Owner CHEN STONE GUANGZHOU CO LTD
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