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A kind of preparation method of high-purity trigonine

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

Active Publication Date: 2021-04-27
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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  • A kind of preparation method of high-purity trigonine
  • A kind of preparation method of high-purity trigonine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029]Take 191 g of N-benzyl diethylethylene amine, 103 g of divintrine, 1200 ml of tetrahydrofuran, 20 g of calcium chloride, 10 g 10% palladium carbon to add 2000 ml of reaction flask, and the gas is transferred at 10 ° C for 5 h, and the GC detection reaction is completed. The filtration was filtered, and the filtrate was often pressed back to the tetrahydrofuran to add 1500 ml of toluene, recrystallized, 50 ° C under reduced pressure, and obtained 160.3 g, yield 93.0%, purity 99.5%.

Embodiment 2

[0031]Take 382 g of N-benzyl diethylene amine, 225 g of divinite, 2000 ml 2-methyl tetrahydrofuran, 50 g of potassium carbonate, 30 g 5% palladium carbon carbon carbon carbonate added 5000 ml of reaction bottle, and reacting hydrogen at 15 ° C for 4 h, GC detection After the reaction was completed, filtration, the filtrate was often pressed back to 2-methyl tetrahydrofuran and added 2500 ml of toluene, recrystallized, 50 ° C under reduced pressure was dried to obtain a product 327.1 g, and the yield was 94.9%, purity 99.3%.

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Abstract

The invention discloses a preparation method of high-purity trigonine. The present invention uses diethylenetriamine and N-benzyldiacetaldehyde amine as main raw materials, adds desiccant, absorbs the water produced, promotes the generation of imine, and at the same time feeds hydrogen to quickly reduce imine to avoid the decomposition of imine. The reaction is more thorough. The method has the advantages of simple steps, low cost, high yield, low requirement on equipment, environmental protection and suitability for industrialized production.

Description

Technical field[0001]The present invention relates to a preparation method of high purity wheels, belongs to the field of medical technology.Background technique[0002]Ring Fuji Ning (1,4,7,10-tetraza-heterointertane) is a very important synthetic diagnostic reagent and a pharmaceutical synthesis intermediate. It is used to remove the inner stones in the human body, inhibit the loss caused by myocardial ischemia reperfusion, especially the precursor of the large ring chelating agent of the synthetic metal ion, can form a very stable complex with ions, for example for synthetic angiography. The binder is alcohol, boridium, and the cranote and spinal magnetic resonance imaging can accurately determine the exact position of the lesion such as tumors. There is a huge potential in the field of medical research, the prospects are broad. Wheel ring Fuji Ning, the structural formula is as follows:[0003][0004]Currently, the method of synthetic cyclic Fuji Ning has the following:[0005]1, STETT...

Claims

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Application Information

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Patent Type & Authority Patents(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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