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Method for preparing dialkyl phenyl-phosphonite

A technology of dialkyl phenyl phosphinate and dialkyl phenyl phosphinate, which is applied in the field of intermediate preparation, can solve the problems of difficult separation, high cost, and easy formation of yellow by-products, etc., so as to improve the conversion The effect of increasing the rate and yield and reducing the production cost

Inactive Publication Date: 2009-09-23
CHANGZHOU VOCATIONAL INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The reaction of phenylphosphine dichloride and amine compounds is easy to generate yellow by-products;
[0006] (2) The yellow by-product is miscible with the product, causing subsequent separations to be very difficult;
[0007] And the second kind of synthetic route of the second step reaction is to use the active metal or the organic compound of active metal with higher price as catalyst, and the cost is relatively high

Method used

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  • Method for preparing dialkyl phenyl-phosphonite
  • Method for preparing dialkyl phenyl-phosphonite
  • Method for preparing dialkyl phenyl-phosphonite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Synthesis of embodiment 1 dimethyl phenylphosphonite

[0040] (1) Synthesis of phenylphosphine dichloride

[0041] Add 0.1mol of benzene and 0.3mol of phosphorus trichloride into a 250mL four-necked flask equipped with an electric liquid-sealed stirring device, a constant pressure dropping funnel, a thermometer, and a spherical condenser (the upper part is equipped with a drying tube and a gas absorption tube). , Aluminum trichloride 0.14mol, reflux reaction under stirring until no hydrogen chloride is released (about 5h of reaction). After the reaction was stopped, 0.13 mol of phosphorus oxychloride was evenly added dropwise from the constant pressure funnel to the four-neck flask under stirring, and the dropping time was controlled at 30 min. Then add 45mL petroleum ether, stir and reflux for 30min. After cooling to room temperature, filter under reduced pressure, distill petroleum ether from the filtrate under normal pressure, and distill under reduced pressure to ...

Embodiment 2

[0045] The synthesis of embodiment 2 diethyl phenyl phosphinates

[0046] (1) The synthesis of phenylphosphine dichloride is the same as the first step of Example 1.

[0047] (2) Synthesis of diethyl phenylphosphonite

[0048] Add 0.4mol absolute ethanol to a 250ml four-necked flask equipped with an electric liquid-sealed stirring device, a constant pressure dropping funnel, a thermometer and a spherical condenser (drying tube is installed on the upper part). Add 0.1mol phenylphosphine dichloride dropwise to the constant pressure dropping funnel under stirring, utilize ice-water bath and adjust the rate of addition of phenylphosphine dichloride, control the reaction temperature at about 0°C, after the dropwise addition, within about Stir at 45°C for 2.5h. After the reaction was completed, the reaction solution was poured into a beaker to cool, and filtered to obtain a solid crude product of diethyl phenylphosphinate, which was recrystallized from a mixed solution of petroleum ...

Embodiment 3

[0049] The synthesis of embodiment 3 phenylphosphonite ethylene glycol

[0050] (1) The synthesis of phenylphosphine dichloride is the same as the first step of Example 1.

[0051] (2) Synthesis of ethylene glycol phenylphosphonite

[0052] Add 0.1 mol of anhydrous ethylene glycol to a 250 ml four-necked flask equipped with an electric liquid-sealed stirring device, a constant pressure dropping funnel, a thermometer and a spherical condenser (with a drying tube on the upper part). Add 0.1 mol of phenylphosphine dichloride dropwise to the constant pressure dropping funnel under stirring, control the reaction temperature at about 5°C by using an ice-water bath and adjusting the addition rate, and stir at about 45°C for 3 hours after the dropwise addition. After the reaction was completed, the reaction solution was poured into a beaker to cool, and filtered to obtain a solid crude product of ethylene phenylphosphinate, which was recrystallized from a mixed solution of petroleum ...

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Abstract

The invention relates to a method for preparing dialkyl phenyl-phosphonite which is a key intermediate of acyl phosphate photoinitiator. The method takes benzene, phosphorus trichloride and alcohol as main materials and synthesizes dialkyl phenyl-phosphonite through a two-step reaction. The method has the improvements that: in the second step of reaction, phenyldichlorophosphine reacts with the alcohol to synthesize the object under the condition of non-catalyst, the reaction temperature is controlled within 10 DEG C below zero to 10 DEG C, and phenyldichlorophosphine is dropwise added; and then the reaction is carried out under the condition of stirring at the temperature of 30 to 50 DEG C for 0.5 to 7 hours. The invention has the advantages of low cost, easy post treatment, high yield, and the like and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of an intermediate of an acyl phosphine oxide photoinitiator, more particularly to a preparation method of an important intermediate of an acyl phosphine oxide photoinitiator-dialkyl phenylphosphinate. Background technique [0002] Dialkyl phenyl phosphinate is an important intermediate for the synthesis of acylphosphine oxide photoinitiators. The preparation method of known dialkyl phenyl phosphinate is completed by two-step reaction usually: the first step prepares phenyl phosphine dichloride earlier, and the second step is by the phenyl phosphine dichloride that the first step makes and Alcohol reaction to prepare dialkyl phenylphosphonites. The first step prepares the synthetic method of phenylphosphine dichloride to have multiple, as: 1) triphenylphosphine and phosphorus trichloride effect; 2) be raw material and phosphorus trichloride reaction with phenylmercury; 3) three Phosphorus chloride reacts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/48C07F9/6571
Inventor 陈炳和赵辉爽丁敬敏
Owner CHANGZHOU VOCATIONAL INST OF ENG
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