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Dibenzyl phosphinic acid synthetic method

A technology of dibenzylphosphinic acid and dibenzyl, applied in the field of synthesizing dibenzylphosphinic acid, can solve the problems of low product purity, complex raw materials, low yield, etc., achieve large extraction capacity and reduce side reactions , the effect of increasing the reaction yield

Inactive Publication Date: 2013-05-01
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0026] These methods have obvious disadvantages, either the raw materials are complicated, or the yield is not high, or the product purity is not high, and a large amount of solvent needs to be used, etc.

Method used

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  • Dibenzyl phosphinic acid synthetic method
  • Dibenzyl phosphinic acid synthetic method
  • Dibenzyl phosphinic acid synthetic method

Examples

Experimental program
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Effect test

Embodiment 1

[0058] Put 1.32 g (0.055 mol) magnesium bar in a 250 mL three-necked flask equipped with stirring, reflux condenser and dropping funnel, immerse the magnesium bar with a small amount of anhydrous ether, and add a small grain of iodine. Add 5.8 mL (0.05 mol) of benzyl chloride and 24 mL of anhydrous ether to the dropping funnel and mix well. The oil bath was heated to about 40-50 °C, and about 1 / 10 of the total amount (about 3 ml) of benzyl chloride anhydrous ether solution was slowly added dropwise. When the temperature of the system rises and starts to reflux, start stirring, slowly add the remaining benzyl chloride solution, control the dripping speed to keep the reaction liquid in a slightly boiling state, and after the dripping is completed, wait for the reaction to stop, cool the reaction bottle slightly, and start the dripping. Slowly add a mixture of 2.8 mL (0.022 mol) diethyl phosphite and 30 mL of anhydrous ether into the liquid funnel (control the dripping speed and ...

Embodiment 2

[0060] Put 9.3 g (0.387 mol) magnesium bar in a 250 mL three-necked flask equipped with stirring, reflux condenser and dropping funnel, immerse the magnesium bar with a small amount of anhydrous ether, and add a small grain of iodine. Add 40.5 mL (0.352 mol) of benzyl chloride and 96 mL of anhydrous ether to the dropping funnel and mix well. The oil bath was heated to about 40-50 °C, and about 1 / 10 of the total amount (about 15 ml) of benzyl chloride anhydrous ether solution was slowly added dropwise. When the temperature of the system rises and starts to reflux, start stirring, slowly add the remaining benzyl chloride solution, control the dripping speed to keep the reaction liquid in a slightly boiling state, and after the dripping is completed, wait for the reaction to stop, cool the reaction bottle slightly, and start the dripping. Slowly add a mixture of 11.3 mL (0.088 mol) diethyl phosphite and 120 mL anhydrous ether into the liquid funnel (control the dripping speed and...

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Abstract

The invention relates to a preparation method of dibenzyl phosphinic acid. The method comprises the following steps: after performing reaction on diethyl phosphite and a Grignard reagent in anhydrous ether, carrying out acidified hydrolysis to obtain dibenzyl phosphine oxide; after purifying the dibenzyl phosphine oxide, placing the dibenzyl phosphine oxide in mixed solution of carbon tetrachloride and water to perform reflux reaction so as to obtain the dibenzyl phosphinic acid. According to the invention, the optimal reaction conditions are obtained by changing conditions of a charging manner, a charge rate, quantity of a solvent and the like, the side reaction is reduced as far as possible and the reaction yield is improved.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to a method for synthesizing dibenzylphosphinic acid. Background technique [0002] In recent years, hydrocarbyl phosphinic acid and its derivatives have been widely used in hydrometallurgy, synthesis of pharmaceutical intermediates, environmental protection, flame retardants and other fields. For example, bis(2,4,4-trimethylpentyl)phosphonic acid (Cyanex 272), which was synthesized by Robertston A.J. in 1983, has been widely used in industry as an efficient extractant for rare metal separation. [0003] Cyanex 272 has unmatched extraction and separation performance for nickel and cobalt extractants such as P507 and P204; Cyanex 272 does not contain ester oxygen atoms, which makes its Pk a It is higher than P507 and P204, so that the acidity of the aqueous phase required for extraction is lower, and the back extraction is easier; in addition, the steric hindrance effect in the molecul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 李林艳蔡妍徐晓庆
Owner TSINGHUA UNIV
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