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A kind of preparation method of α-hydroxy phosphate

A technology of α-hydroxy phosphonate and diethyl phosphite, which is applied in the field of preparation of phosphorus-containing compounds, can solve the problems of large amount of catalyst, harsh reaction conditions of catalyst, and no reports of diethyl phosphite reaction, etc. Wide range of effects

Active Publication Date: 2018-01-09
SUZHOU UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

However, the existing catalysts have defects such as harsh reaction conditions and large catalyst consumption; in the prior art, there are few reports on the application of double β-diimine divalent rare earth complexes with β-diimine as ligands, and even more There is no report on the reaction of carbonyl compounds and diethyl phosphite catalyzed by bis-β-diimino divalent ytterbium complexes

Method used

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  • A kind of preparation method of α-hydroxy phosphate
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Embodiment

[0019] Example Yb(L 2-Me ) 2 (THF) Catalytic Synthesis of α-Hydroxy Phosphate from Ketone and Diethyl Phosphite

[0020] According to the raw material composition of Table 1 and process parameter, in glove box, add diethyl phosphite with pipette gun under nitrogen protection in the reaction flask of 20mL, then add catalyst Yb (L 2-Me ) 2 (THF), then stirred at room temperature, then added the ketone with a pipette gun, after reacting at room temperature, sucked a drop into the NMR tube with a dropper, and added CDCl 3 Make a solution, calculate 1 H spectrum yield. Transferred out of the glove box, terminated the reaction with ethyl acetate, dissolved with an appropriate amount of ethyl acetate, and removed the solvent by rotary evaporation, and the remaining solid was washed with n-hexane (4×5 mL) to obtain the corresponding α-hydroxyphosphate.

[0021] Table 1 The molar ratio of raw materials and process parameters for the synthesis of α-hydroxyphosphate

[0022] .

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Abstract

The invention provides a preparing method of alpha-hydroxy phosphate. The method specifically comprises: in an nitrogen gas atmosphere, using ketone and diethyl phosphite as reactants to prepare the structure-diversified alpha-hydroxy phosphate under catalyzing of an organic complex. According to the preparing method, the reaction of the ketone and the diethyl phosphate can be catalyzed with high activity under mild conditions, and the method has the advantages of short reaction time, mild reaction conditions, and convenient and simple posttreatment method.

Description

technical field [0001] The invention relates to a preparation technology of phosphorus-containing compounds, in particular to a preparation method of α-hydroxy phosphate. Background technique [0002] As a class of phosphorus-containing compounds, α-hydroxyphosphate is an important component of some antiviral agents, anticancer drugs, and enzymes, and has a variety of biological functions. At the same time, the compound has a wide range of applications in the cutting-edge molecular science fields, such as polymer materials, nanotechnology, biological detection, drug development and asymmetric catalysis; the compound can also be further synthesized derivatives with more complex structural units (See: Karasik, A. A.; Sinyashin, O. G. Phosphorus Compounds: Advanced Tools in Catalysis and Material Science. Vol.37, Eds.: Peruzzini, M.; Gonsalvi, L, Kazan, 2011, pp. 375-444.; Sikorski, J.A.; Miller, M. J.; Braccolino, D. S. Phosphorus, Sulfur and Silicon . 1993, 76 , 115). [...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40
CPCC07F9/4006
Inventor 薛明强刘倩倩沈琪洪玉标郑煜
Owner SUZHOU UNIV