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Preparation method of high-purity cycleanine

A high-purity technology with ring vines, applied in the field of medicine, can solve the problems of high price, inconvenient use, and unsuitability for industrial production of lithium tetrahydrogen, and achieve the effects of less impurities, avoiding the use of sulfuric acid, and short reaction time

Active Publication Date: 2020-03-27
SHANDONG BOYUAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, lithium aluminum tetrahydrogen is expensive and decomposes explosively when it meets water. It is extremely inconvenient to use and is not suitable for industrial production.

Method used

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  • Preparation method of high-purity cycleanine
  • Preparation method of high-purity cycleanine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 191g of N-benzyldiacetaldehyde amine, 103g of diethylenetriamine, 1200ml of tetrahydrofuran, 20g of calcium chloride, 10g of 10% palladium carbon into a 2000ml reaction bottle, pass in hydrogen gas and react at 10°C for 5h, after the reaction is detected by GC, After suction filtration, the filtrate recovered tetrahydrofuran under normal pressure, then added 1500ml of toluene, recrystallized, and dried under reduced pressure at 50°C to obtain 160.3g of the product, with a yield of 93.0% and a purity of 99.5%.

Embodiment 2

[0031] Take 382g of N-benzyldiacetaldehyde amine, 225g of diethylenetriamine, 2000ml of 2-methyltetrahydrofuran, 50g of potassium carbonate, 30g of 5% palladium carbon into a 5000ml reaction flask, inject hydrogen into the reaction bottle at 15°C for 4h, and detect by GC After the reaction was completed, it was filtered with suction, and 2-methyltetrahydrofuran was recovered from the filtrate under normal pressure, then 2500ml of toluene was added, recrystallized, and dried under reduced pressure at 50°C to obtain 327.1g of the product, with a yield of 94.9% and a purity of 99.3%.

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Abstract

The invention discloses a preparation method of high-purity cycleanine. Diethylenetriamine and N-benzyl diacetaldehyde amine are used as main raw materials, a drying agent is added, generated water isabsorbed, the generation of imine is promoted, meanwhile, hydrogen is introduced to rapidly reduce the imine, the decomposition of imine is avoided, and the reaction is more thorough. The method is simple in step, low in cost, high in yield, low in equipment requirement, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of high-purity trigonine, which belongs to the technical field of medicine. Background technique [0002] Trigonine (1,4,7,10-tetraazacyclododecane) is a very important synthetic diagnostic reagent and intermediate in drug synthesis. It is used to remove stones in the human body and inhibit the loss caused by myocardial ischemia-reperfusion, especially as the precursor of macrocyclic chelating agents for the synthesis of metal ions, and can form very stable complexes with ions, such as for synthetic contrast Gadobutrol and gadoteridol can be used for MRI imaging of the brain and spinal cord, which can accurately determine the exact location of tumors and other lesions. It has great potential and broad prospects in the field of medical research. Ring ring tenning, the structural formula is as follows: [0003] [0004] At present, the methods of synthesizing chrysanthemum mainly contain the following k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/02
CPCC07D257/02
Inventor 昝金行李太同赵希伟刘茂盛
Owner SHANDONG BOYUAN PHARM CO LTD
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