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Phosphorus anionic reagent as well as preparation method and application thereof

An anion and reagent technology, applied in the field of phosphorus anion reagents and their preparation, can solve the problems of harsh reaction conditions, large substrate limitations, and large energy consumption, and achieve the effects of loose reaction conditions, low reaction energy, and safe synthesis.

Active Publication Date: 2018-11-30
武汉中科先进材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since most of the reaction substrates used in this method are sensitive to air, the reaction conditions are relatively harsh, the substrates are limited, and the reaction produces a large number of organic halogenated by-products, which do not meet the requirements of green chemical development.
At the same time, the production process of white phosphorus consumes a lot of energy and causes great pollution to the environment.

Method used

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  • Phosphorus anionic reagent as well as preparation method and application thereof
  • Phosphorus anionic reagent as well as preparation method and application thereof
  • Phosphorus anionic reagent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Synthesis of tetrabutylammonium salt of bis(trichlorosilyl)phosphorus anion:

[0035]

[0036] The specific operation is as follows:

[0037] In a glove box filled with inert gas Ar, weigh 339 mg of tetrabutylammonium dihydrogen phosphate (1 mmol) and put it into a high-pressure reactor (pressure 1 MPa), add 10 ml of trichlorosilane, heat to 120 ° C and stir for 48 h, the reaction The liquid was washed with 10 ml of n-hexane and dried to obtain 1.2 g of white powder with a yield of 72%.

[0038] 1 H NMR (400MHz,D 2 O)δ3.27–2.89(m,2H),1.69–1.39(m,2H),1.39–1.12(m,2H),0.83(t,J=7.3Hz,3H).1.00(t,J=7.3 Hz,3H).

[0039] 31 P NMR (162MHz, CDCl 3 )δ-156.

Embodiment 2

[0041] Synthesis of di(dichloroboryl)phosphorus anion tetrabutylammonium salt:

[0042]

[0043] The specific operation is as follows:

[0044] In a glove box filled with inert gas He, weigh 339mg of tetrabutylammonium dihydrogenphosphite (1mmol) and put it into a high-pressure reactor (pressure is 1MPa), add 10ml of butyldichloroborane, heat to 120°C and stir After reacting for 48 hours, the reaction solution was washed with 10 ml of n-hexane and dried to obtain 1.4 g of white powder with a yield of 68%.

[0045] 1 H NMR (400MHz, CDCl 3 )δ3.52–3.29(m,2H),1.79–1.62(m,2H),1.55–1.39(m,2H),1.01(t,J=7.3Hz,3H).

Embodiment 3

[0047] Synthesis of di(dichloroaluminum) phosphorus anion tetrabutylammonium salt:

[0048]

[0049] The specific operation is as follows:

[0050] In a glove box filled with inert gas Ne, weigh 339mg of tetrabutylammonium dihydrogen hypophosphite (1mmol) and put it into a high-pressure reactor (pressure is 1MPa), add 5g of ethyl aluminum dichloride, and heat 10ml of tetrahydrofuran to 120°C After stirring for 48 hours, the reaction solution was washed with 10 ml of n-hexane and dried to obtain 1.05 g of yellow powder with a yield of 57%.

[0051] Elemental Analysis C 16 h 36 Cl 4 N 1 P 1 Al 2 : Calculated C 40.94, H 7.75, N 3.03, Theoretical C 40.96, H 7.73, N 2.99.

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Abstract

The invention discloses a phosphorus anionic reagent as well as a preparation method and application thereof. The phosphorus anionic reagent has the structural formula as shown in the figure I in thespecification, wherein X is any one of elements of aluminum, boron, silicon and titanium, the valence state of X is m, Z is halogen or pseudohalogen, and n is equal to m-1, R<+> is any one of an ammonium positive ion, a sulfur onium ion and a phosphorus onium ion. The preparation method comprises the following step that under the protection of inert gas, a phosphoric acid derivative reacts with areducing agent in an organic solvent so as to prepare the phosphorus anionic reagent, wherein the reducing agent has the structural formula as shown in the figure II in the specification, and in the structural formula of the reducing agent, R1 is any one of hydrogen, C1-6 alkyl, C1-3 alkoxy, phenyl and substituted phenyl. According to the phosphorus anionic reagent as well as the preparation method and application thereof, the preparation process of the phosphorus anionic reagent is simple, the obtained phosphorus anionic reagent is high in activity and can be applied to prepare a compound containing any one or more of chemical bonds such as a P-C bond, a P-S bond, a P-F bond and a P-H bond, the range of synthesized phosphorus compounds is wide, the use of phosphorus trichloride can be avoided, and the the phosphorus anionic reagent as well as the preparation method and application thereof are green, environmentally friendly, safe and efficient.

Description

technical field [0001] The invention relates to the technical field of ion reagents, in particular to a phosphorus anion reagent and its preparation method and application. Background technique [0002] Organophosphorus compounds are an important class of organic compounds, widely used in pesticides, fertilizers, battery electrolytes, flame retardants, plasticizers, water quality stabilizers, petroleum additives and surfactants, etc. field exhibited excellent performance. In addition, phosphorus compounds play an extremely important role in the synthesis of new substances. Many major breakthroughs in organic synthesis are closely related to the discovery of new organophosphorus reagents, phosphorus ligands and phosphorus catalysts. [0003] The traditional preparation method of organophosphorus compounds is mainly obtained through the nucleophilic substitution reaction of phosphorus trichloride, while phosphorus trichloride is mainly synthesized by a high-energy-consuming ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/08C01B33/08C07F9/50C07F9/06C01D13/00
CPCC01B25/08C01B25/084C01B25/085C01B33/08C01D13/00C07F9/06C07F9/5031C07F9/5077C07F9/5081
Inventor 喻学锋吴列
Owner 武汉中科先进材料科技有限公司
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