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A kind of preparation method of high-purity trigonine

The technology of a tertenin and compound is applied in the field of preparation of high-purity terranine, which can solve the problems of expensive raw material dithiooxalic acid, low comprehensive yield, and few steps, and achieve good development prospects and low cost. The effect of low and three wastes

Inactive Publication Date: 2016-03-30
厦门市华兴化工有限公司
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Problems solved by technology

Although this method has only three steps, the yield is not low, but the raw material dithiooxalic acid is relatively expensive
The cyclization yield of diethyl oxalate condensation method is not high, so the comprehensive yield is low
The oxalic acid condensation method reacts with oxalic acid aqueous solution and triethylenetetramine (TETA) to generate a tricyclic intermediate, and then expands the ring with 1,2-dibromoethane (EDB), and obtains cyclen by oxidative hydrolysis, but this The raw materials of the method are easy to obtain, there are not many steps, and the overall yield is not low, but the disadvantage is that the oxidation and hydrolysis reactions need a long time, and high-pressure hydrolysis is also required

Method used

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  • A kind of preparation method of high-purity trigonine
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  • A kind of preparation method of high-purity trigonine

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Embodiment 1

[0087] Embodiment 1: the preparation of trigonine

[0088] first step:

[0089] Add 195g (1.03mol) of TETA hydrate to a 2000ml four-necked bottle with a thermometer, add 750ml of drinking water and 150ml of ethanol, under stirring, add 110g (1.9eq) of magnesium hydroxide under nitrogen gas, and then cool to -5 degrees. Add dropwise glyoxal aqueous solution (145g 40% glyoxal, 400mL water and 100ml ethanol) (1.0eq), add dropwise for 2 hours, keep at -5°C for 2 hours after addition, filter with air (spread a layer of silicon bath soil) , the solid was washed once with a small amount of water, the filtrate and washings were combined, the filtrate was concentrated under reduced pressure with a rotary evaporator to obtain a dry residue, the residue was added to 150ml of toluene to separate water, and anhydrous potassium carbonate was added to dry to obtain a light yellow oil compound B .

[0090] Step two:

[0091] Add 152g (4.50eq) of anhydrous sodium carbonate, 21.6g (0.45eq) o...

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Abstract

The invention provides a preparation method of high-purity cyclen. The method comprises the following preparation paths. Cyclen obtained by the method of the invention has high purity. At the same time, the method greatly reduces the energy consumption and the power cost, and thereby reducing the raw material cost; the method greatly improves the reaction rate, reduces the catalyst amount and the reaction temperature, thereby shortening the consuming time of the process, and reducing the process cost; and the method greatly reduces the acid amount consumption, and thereby greatly reducing the equipment loss. The preparation method improves the production efficiency, and enables the product quality to reach more than 99.8%; hydrazine hydrate is used for replacing diethylenetriamine for a hydrolysis reaction, so the process is suitable for industrialized production. The method of the invention is environmentally friendly, is cost-saving, and is suitable for environment-friendly industrialization.

Description

technical field [0001] The invention relates to the field of polymer synthesis chemistry, in particular to a preparation method of high-purity trigonine. Background technique [0002] Luhuan Tengning (1,4,7,10-tetraazadodecane, cyclen) can be used as a scavenging drug for human stones, and as a mimic of MnSOI, it can inhibit the damage caused by myocardial ischemia-reperfusion, and has anti- AIDS activity, etc., especially in the manufacture of contrast agents for magnetic resonance imaging (MRI), X-ray, CT, ultrasound imaging and other medical imaging technologies, as well as radioactive drugs for malignant tumors, have shown extremely important application value. Its derivatives are used to form complexes with DOTA, which can be used in radioimmunotherapy when linked to monoclonal antibodies. The complexes formed with lanthanides are widely used in biomedicine as Na, NMR ultrafine shifting reagents. Now that the aging population in the world is getting more and more serio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/02
Inventor 陈国强赖启明李满园
Owner 厦门市华兴化工有限公司
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