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Asymmetric phosphorus oxide pyridine triazine derivative and synthesis method thereof

A technology of phosphorus oxide pyridine triazines and synthetic methods, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., capable of solving trivalent minor actinide ions and lanthanide ions Separated from each other, etc., to achieve good application prospects, strong extraction ability, and the best effect of extraction ability

Pending Publication Date: 2022-05-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, o-phenanthroline phosphorus oxide cannot separate trivalent minor actinide ions and lanthanide ions from each other

Method used

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  • Asymmetric phosphorus oxide pyridine triazine derivative and synthesis method thereof
  • Asymmetric phosphorus oxide pyridine triazine derivative and synthesis method thereof
  • Asymmetric phosphorus oxide pyridine triazine derivative and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Ph 2 Synthesis of CA-TPPO

[0045] Step 1: Put 2.5g of 6-bromo-2-cyanopyridine and 10.0ml of hydrazine monohydrate into a reaction flask, add 10.0mL of deionized water and react at 25°C for 1.0h. After the reaction, the solid powder was filtered directly, washed three times with deionized water, and then dried overnight at 60° C. to obtain intermediate product 2, about 2.0 g.

[0046]

[0047] Step 2, 2.3g of camphorquinone is dissolved in ultra-dry ethanol or tetrahydrofuran, and is added dropwise to the ultra-dry ethanol suspension solution containing 2.0g of brominated monopyridylamine hydrazone (intermediate product 2 prepared in step 1) through a constant pressure funnel, , and react after the dropwise addition is completed. The reaction was first refluxed for 3 h under the protection of high-purity argon, and then stirred overnight at room temperature. The reaction was tracked by TLC until the reaction of the raw materials was complete.

[0048] Obta...

Embodiment 2

[0059] Synthesis of Example 2 BuPhCA-TPPO

[0060] Take 1g of the intermediate product 4 prepared in step 2 of Example 1, dissolve it with 0.8g butylphenylphosphine oxide in 50.0mL ultra-dry toluene solution and add 28.0mg (0.122mmol) of palladium acetate to the solution, dppf 1, 160.0mg (0.244mmol) of 1'-bis(diphenylphosphino)ferrocene and 3.0g of cesium carbonate were vacuumized under the protection of argon, and refluxed at 110°C for 24h. After the reaction was completed, the solvent toluene was removed by suction filtration and rotary evaporator. Dichloromethane and saturated NaCl solution were added to the crude product, and the organic phase was combined after washing and extraction several times to obtain a brown oil, which was treated with dichloromethane / ethyl acetate / methanol (v / v / v=30:30:1) After separation by column chromatography as an eluent, 0.8 g of the product BuPhCA-TPPO brown oil was obtained.

[0061]

[0062] (1) BuPhCA-TPPO 1 H NMR characterization ...

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Abstract

The invention relates to the technical field of organic synthesis, and discloses an asymmetric phosphorus oxide pyridine triazine derivative and a synthesis method thereof.The asymmetric phosphorus oxide pyridine triazine derivative has the structural formula shown in the formula I. The synthesis method comprises the steps that 1, halogenated-2-cyanopyridine and hydrazine monohydrate react to obtain an intermediate product A; step 2, dropwise adding the intermediate product A into a camphorquinone solution, carrying out a reaction to obtain a filtrate, carrying out spin-drying, and purifying to obtain an intermediate product B; and 3, dissolving the intermediate product B and phosphorus oxide in a solution, and reacting to obtain the derivative, the derivative has the advantages of stable performance, strong acid hydrolysis resistance, high extraction capacity, high extraction rate and the like, and has a good application prospect in the field of co-extraction separation of trivalent lanthanide series and actinide series in nuclear industry waste liquid, especially high-level liquid waste.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to an asymmetric oxidized phosphopyridine triazine derivative and a synthesis method thereof. Background technique [0002] The effective treatment and disposal of nuclear fuel is a key factor to ensure the sustainable development of nuclear energy, especially the separation of actinide elements with long-term strong radioactivity. The PUREX process (PUREX, Plutonium Uranium Reduction EXtraction) currently adopted internationally can separate and recycle most of the uranium and plutonium (accounting for about 95% of the total spent fuel) in spent fuel. The waste liquid produced after the separation of uranium and plutonium, in which the concentration of nitric acid is 3-4M, is also called high active liquid waste (HLW), which still contains long-lived minor actinides (such as Am(III), Cm(III)) is the main source of long-term radioactivity and radiation toxicity of high-le...

Claims

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Application Information

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IPC IPC(8): C07F9/6558C22B3/36C22B59/00C22B60/02G21F9/12
CPCC07F9/65583C22B59/00C22B60/0295G21F9/125Y02W30/50
Inventor 徐雷肖成梁余志扬
Owner ZHEJIANG UNIV
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