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Asymmetric dithiophosphinic acid synthesis method

A technology of dithiophosphinic acid and synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry and other directions, and can solve problems such as lack of synthesis methods.

Active Publication Date: 2010-01-06
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Recently it has been reported that Grignard reagent and thion trichloride P(S)Cl 3 The reaction generates a biphosphine intermediate, which is then thiolyzed and acidified into a symmetrical dialkyldithiophosphinic acid, but there is no such thing as asymmetrical dithiophosphinic acid synthesis methods for substituents.

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  • Asymmetric dithiophosphinic acid synthesis method

Examples

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Embodiment 1

[0044] The synthesis of embodiment 1 o-trifluoromethylphenyl (octyl) dithiophosphinic acid

[0045] The first step, preparation of organometallic reagent ①

[0046] In this example, organometallic reagent ① uses organozinc reagent;

[0047] (1), preparation of Grignard reagent octylmagnesium bromide

[0048] Under the protection of argon, add 0.525mol magnesium strips Mg12.778g and anhydrous ether 25mL into the three-neck flask according to the weight volume ratio of 1:1.95, then add 0.05g of iodine particles; add 2~3mL of n-octyl bromide Alkane C 8 h 17 Br (87.0mL, 0.5mol) ether (275mL) solution to the three-necked reaction flask to initiate the reaction, n-octane bromide C 8 h 17 The volume ratio of Br to anhydrous ether is 1:3.16; while stirring, add bromo-n-octane C 8 h 17 Br ether solution, after the dropwise addition is completed, continue to heat to 30-40°C and reflux until the magnesium bars disappear;

[0049] (2), the obtained brown-black clear liquid, that i...

Embodiment 2

[0065] The synthesis of embodiment 2 butyl octyl dithiophosphinic acid

[0066] The first step, preparation of organometallic reagent ①

[0067] In this example, organometallic reagent ① uses organozinc reagent;

[0068] (1), preparation of Grignard reagent octylmagnesium bromide

[0069] Under the protection of argon, add 0.42 mol of magnesium strips Mg10.0g and anhydrous ether 10mL into the three-neck flask according to the weight volume ratio of 1:1, then add 0.05g of iodine particles; add 2~3mL of n-octyl bromide Alkane C 8 h 17 Br (69.4mL, 0.4mol) ether (210mL) solution to the three-necked flask to initiate the reaction, n-octane bromide C 8 h 17 The volume ratio of Br to anhydrous ether is 1:3.04; while stirring, add brominated n-octane C 8 h 17 Br ether solution, after the dropwise addition is completed, continue to heat to 30-40°C and reflux until the magnesium bars disappear;

[0070] (2), the obtained brown-black clear liquid, that is, the Grignard reagent, w...

Embodiment 3

[0086] The synthesis of embodiment 3 o-trifluoromethylphenyl (phenyl) dithiophosphinic acid

[0087] The first step, organometallic reagent ① preparation

[0088] In this example, organometallic reagent ① uses Grignard reagent;

[0089] Preparation of Grignard Reagent Phenylmagnesium Bromide

[0090] Under the protection of argon Ar, add 0.105mol magnesium strips Mg2.553g and anhydrous ether 5mL into the three-neck flask according to the weight volume ratio of 1:1.99, then add 0.05g of iodine particles; dropwise add 2~3mL of bromobenzene C 6 h 5 Br (10.5mL, 0.1mol) diethyl ether (35mL) solution to the three-necked flask to initiate the reaction, bromobenzene C 6 h 5 The volume ratio of Br to anhydrous ether is 1:3.33; add bromobenzene C dropwise while stirring 6 h 5 Br ether solution, after the dropwise addition is completed, continue to heat to 30-40°C and reflux until the magnesium bars disappear;

[0091] The second step, phenyl phosphorus dichloride C 6 h 5 PCl 2...

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Abstract

An asymmetric dithiophosphinic acid synthesis method comprises the following steps: adopting phosphorus trichloride as raw material to react with organic metal reagent RMX, producing asymmetric dihydroxylphosphorus chloride, then obtaining phosphinic acid by reacting the asymmetric dihydroxylphosphorus chloride, sulphur and sodium bisulfide, purifying the corresponding salt by column chromatography or recrystallization and finally obtaining asymmetric dithiophosphinic acid by converting. The method can be used in the preparation field of dithiophosphinic acid extractant compounds.

Description

technical field [0001] The invention belongs to the preparation technology of dithiophosphinic acid extractant compounds, and mainly relates to a synthesis method of unsymmetrical dithiophosphinic acid. Background technique [0002] The development of advanced nuclear fuel cycle technology is the basis for ensuring the sustainable development of nuclear energy in my country, and the separation technology of high-level radioactive waste liquid is one of the cores of advanced nuclear fuel cycle technology. The goal of the high-level waste liquid separation process is to separate the actinides from the high-level waste liquid. In the existing separation process, because the chemical properties of trivalent actinides and lanthanides are very similar, they are separated into the same stream. In order to realize the transmutation of trivalent actinides and non-alphalation of lanthanide wastes, it is necessary to further separate trivalent actinides from lanthanides. Since dithio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 王芳贾彩何喜红陈靖
Owner TSINGHUA UNIV
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