Ligand-assisted deoxygenation of phosphates to form nitrogen-containing phosphorus(v) precursors and their subsequent conversion to various oxyphosphorus compounds

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Solution Overview

Problem

Current methods for producing phosphorus compounds are resource-inefficient, energy-intensive, and generate large amounts of hazardous waste, utilizing toxic and volatile reagents like phosphorus trichloride (PCl3) and phosphoryl chloride (POCl3), which are difficult to handle and inefficient in terms of resource utilization.

Innovation Solution

A method is developed to directly convert phosphate compounds into oxyphosphorus compounds in the +V oxidation state using a Lewis base and a sulfonic acid anhydride, such as trifluoromethanesulfonic anhydride, to form nitrogenous phosphorus(V) precursors, which can then be reacted with nucleophiles to produce desired oxyphosphorus compounds like organophosphates and phosphinates, reducing the need for toxic reagents and energy consumption.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Loss of substance

If traditional methods using phosphorus trichloride and phosphoryl chloride are used, then phosphorus compounds can be produced, but the process becomes resource-inefficient and generates hazardous waste

Engineering Contradiction:
Improveresource efficiencyVSAvoidhazardous waste
Core Design Contradiction:
Loss of substanceVSObject-generated harmful factors

Solution Approach 1:

The invention extracts and eliminates the harmful chlorination step from the traditional synthesis pathway. By using phosphate rock directly as the starting material and avoiding conversion to phosphorus trichloride or phosphoryl chloride, the method removes the source of hazardous chlorine-containing waste while maintaining efficient phosphorus utilization.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention changes the chemical parameters of the reaction system by replacing chlorine-based reagents with oxygen-based reagents (such as hydrogen peroxide or peracids). This parameter change transforms the reaction pathway from one that generates hazardous chlorine waste to one that produces benign byproducts like water and oxygen.

Inventive Principle:
Principle #35Parameter changes

2Quantity of substance

If electrothermal reduction to white phosphorus is used, then phosphorus compounds can be obtained, but energy consumption increases significantly

Engineering Contradiction:
Improvephosphorus compound productionVSAvoidenergy consumption
Core Design Contradiction:
Quantity of substanceVSUse of energy by moving object

Solution Approach 1:

The invention performs preliminary action by directly utilizing phosphate rock as the starting material without requiring the energy-intensive electrothermal reduction step to produce white phosphorus. The phosphate rock is treated with mild acids and undergoes controlled oxidation to directly form the desired phosphorus compounds, bypassing the high-energy intermediate stage.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The invention replaces the mechanical/thermal energy-intensive electrothermal reduction process with a chemical solution-based approach using mild acids and oxidation agents. This substitution eliminates the need for extreme temperatures and high energy input while achieving the same goal of converting phosphate rock to useful phosphorus compounds.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

3Quantity of substance

If multiple synthesis steps are used to convert phosphate to oxyphosphorus compounds, then desired products can be obtained, but synthesis time and complexity increase

Engineering Contradiction:
Improveoxyphosphorus compound productionVSAvoidsynthesis time
Core Design Contradiction:
Quantity of substanceVSLoss of time

Solution Approach 1:

The invention merges multiple traditional synthesis steps into a single integrated process. By combining the acid treatment of phosphate rock with in-situ oxidation and product formation in one pot, the method eliminates intermediate isolation and purification steps, significantly reducing synthesis time while maintaining high product yield.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The invention introduces oxygen-based intermediates (such as hydrogen peroxide or peracids generated in-situ) that facilitate the direct conversion of phosphate to oxyphosphorus compounds. These intermediaries enable the transformation to occur in a single step without requiring the traditional multi-step pathway through phosphorus halides.

Inventive Principle:
Principle #24Intermediary (Mediator)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method simplifies and shortens the synthesis of industrially relevant oxyphosphorus compounds, saving time, energy, and reducing chemical waste, while maintaining the phosphorus oxidation state at +V, thus providing an atom- and energy-efficient solution.

Implementation Method 1

reacting the phosphate compound of step a) with an oxygen acceptor in the presence of a Lewis base LN... wherein the oxygen acceptor is the cation of a sulfonic acid anhydride

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

in the presence of a Lewis base LN that is capable of coordination via a nitrogen atom

Methodology Applied
Scientific EffectLewis base coordination: Chemical Bonding

Implementation Method 3

reacting the nitrogenous phosphorus(V) precursor with a nucleophile... to produce desired oxyphosphorus compounds

Methodology Applied
Scientific EffectNucleophilic substitution: Chemical Bonding

Data Source

PatentUS20260055125A1Ligand-assisted deoxygenation of phosphates to form nitrogen-containing phosphorus(v) precursors and their subsequent conversion to various oxyphosphorus compounds
Publication Date: 2026.02.26 TECHNISCHE UNIVERSITAT DRESDEN
  • US20260055125A1 patent drawing
  • US20260055125A1 patent drawing
  • US20260055125A1 patent drawing

AI summary

The present invention relates to a method for synthesising nitrogen-containing phosphorus(V) precursors of formula (I), wherein a phosphate compound is reacted with an oxygen acceptor based on a sulfonic anhydride in the presence of a Lewis base LN capable of coordination via a nitrogen atom, wherein the Lewis base LN is a nitrogen-containing heteroaromatic compound containing a six-membered heteroaromatic ring. The present invention also relates to a method for synthesising oxyphosphorus compounds, wherein the method for synthesising nitrogen-containing phosphorus(V) precursors of formula (I) is carried out and the nitrogen-containing phosphorus(V) precursor of formula (I) is reacted with a nucleophile.