Water heating synthesis of yttrium-diethyltriamine pentacetate

A technology for diethylenetriaminepentaacetic acid and hydrothermal synthesis, which can be used in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc., and can solve the problems of long reaction time, increased toxicity, and difficulty in separation and other problems, to achieve the effect of less impurities, reducing content and improving reaction efficiency

Inactive Publication Date: 2005-10-12
EAST CHINA NORMAL UNIV
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Problems solved by technology

The existing method of synthesizing gadolinium-diethylenetriaminepentaacetic acid magnetic resonance imaging contrast agent is to use gadolinium chloride as a raw material and add diethylenetriaminepentaacetic acid to prepare it. Since gadolinium chloride is toxic, it is easy to mix in the product. Excess gadolinium ions increase toxicity ([1] Kunimasa J I, Inui KI, Hori R. et al., Mannan-Coated Liposome Delivery of Gadolimium-Diethylentriaminepentaacetic acid, a contrast agent for usein magnetic resonance imaging (gadolimium-pentetic acid mannose Fat, magnetic resonance imaging contrast agent).[J].Chem.Pharm.Bull., 1992.40(9):2565-2567)
The oxide of gadolinium is also used as raw material to prepare, but the reaction time is long, the yield is low, there are many impurities, and the separation is difficult ([2] the patent number and the title are respectively US5560903 and 'Method of enhancing paramagnetism in chelates for MRI' (in magnetic resonance U.S. Patent for Method for Enhancing Paramagnetism with Chelates in Imaging

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In the first step, mix 1 mmol, namely 0.363 g of gadolinium oxide, and 2 mmol, namely 0.787 g of diethylenetriaminepentaacetic acid, and add them into the hydrothermal reactor, and add 55 mmol, namely, 1 g of water. Under the hydrothermal condition of 190°C, heat for 15 minutes, take out the reactor and cool it down.

[0019] In the second step, after the solution prepared in the first step is cooled, filter and evaporate to obtain crystals, the crude product of gadolinium-diethylenetriaminepentaacetic acid;

[0020] Step 3 Recrystallize from ethanol and dry in vacuo to obtain 1.8 mmol of pure gadolinium-DETA.

Embodiment 2

[0022] The first step is to mix 0.1mmol, namely 0.0363g gadolinium oxide and 0.2mmol, namely 0.0787g diethylenetriaminepentaacetic acid, and add them to the hydrothermal reactor, and add 55mmol, namely 1g water. Under the hydrothermal condition of 150°C, heat for 60 minutes, take out the reactor and cool it down.

[0023] In the second step, after the solution prepared in the first step is cooled, filter and evaporate to obtain crystals, the crude product of gadolinium-diethylenetriaminepentaacetic acid;

[0024] Step 3 Recrystallize from ethanol and dry in vacuo to obtain 0.18 mmol of pure gadolinium-DETA.

Embodiment 3

[0026] The first step mixes 0.5mmol, namely 0.182g of gadolinium oxide, and 1mmol', namely, 0.394g of diethylenetriaminepentaacetic acid, and puts them into the hydrothermal reactor, and adds 110mmol, namely, 2g of water. Under the hydrothermal condition of 120°C, heat for 3 hours, take out the reactor and cool it down.

[0027] In the second step, after the solution prepared in the first step is cooled, filter and evaporate to obtain crystals, the crude product of gadolinium-diethylenetriaminepentaacetic acid;

[0028] Step 3 Recrystallize from ethanol and dry in vacuum to obtain 0.9 mmol of pure gadolinium-DETA.

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Abstract

A hydrothermal synthesis of gadolinium-diethylentriaminepentaacetic acid is carried out by using gadolinium oxide and diethylentriaminepentaacetic acid, hydrothermal synthesizing, and obtaining gadolinium- diethylentriaminepentaacetic. It is an inorganic complex chemical synthetic technology. Its advantages include less impurities, high reacting speed and output efficiency.

Description

Technical field [0001] The invention relates to a method for hydrothermally synthesizing gadolinium (Gadolinium, Gd)-diethylenetriaminepentaacetic acid (Diethylentriaminepentaacetic acid, DTPA) magnetic resonance imaging contrast agent (MRI), which belongs to inorganic coordination chemistry The technical field of synthesis. Background technique [0002] Magnetic resonance imaging technology has been widely used in the biological and medical fields, and has become a common medical diagnostic method. A widely used contrast agent for magnetic resonance imaging. The existing method of synthesizing gadolinium-diethylenetriaminepentaacetic acid magnetic resonance imaging contrast agent is to use gadolinium chloride as a raw material and add diethylenetriaminepentaacetic acid to prepare it. Since gadolinium chloride is toxic, it is easy to mix in the product. Excess gadolinium ions increase toxicity ([1] Kunimasa J I, Inui KI, Hori R. et al., Mannan-Coat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00
Inventor 施沈一单永奎
Owner EAST CHINA NORMAL UNIV
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