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A kind of reduction prepares the method for triphenylphosphine

A technology of triphenylphosphine and triphenylphosphine oxide, which is applied in the field of reducing and preparing triphenylphosphine, which can solve the problems of harsh reaction conditions, rare reaction raw materials, and non-renewable reducing agent, and achieve less catalyst amount and high catalytic efficiency , The effect of less catalyst dosage

Active Publication Date: 2020-04-17
江苏富比亚化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned reduction method of triphenylphosphine oxide has the following disadvantages: (1) the raw materials for the reaction are rare and the reaction conditions are harsh; (2) the reducing agent cannot be regenerated and the reduction product is waste, forming secondary pollutants, which is not environmentally friendly and energy-saving. green reduction reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Put 27.8g of triphenylphosphine oxide, 88.2g of diphenylphosphine chloride (the mass ratio of the two is 1:3.17), and 0.56g of trifluoromethanesulfonic acid (triphenylphosphine oxide) into the 250mL reaction flask replaced by nitrogen. 2% of the mass), the temperature is raised to 150°C, and the temperature is kept for 12h. After cooling to room temperature, turn on the vacuum pump. After the vacuum degree reaches 0.098Mpa, the temperature is slowly raised to intercept the mixture of diphenylphosphine chloride and diphenylphosphinyl chloride. After the high boiler is cooled, put in 50g of toluene, wash with saturated sodium carbonate to neutrality, wash the organic layer twice with deionized water, separate the organic layer, distill to recover the toluene, put 30g of ethanol in the bottle, and recrystallize to obtain three Phenylphosphine was 23.6g, the yield was 90%, and the content detected by HPLC was 98.7%.

Embodiment 2

[0045] Put 27.8g of triphenylphosphine oxide, 71.6g of phenylphosphine dichloride (the mass ratio of the two is 1:2.58), 0.56g of trifluoromethanesulfonic acid (triphenylphosphine oxide) into the 250mL reaction flask after nitrogen replacement. 2% of the mass), the temperature is raised to 150°C, and the temperature is kept for 12h. After cooling to room temperature, turn on the vacuum pump. After the vacuum degree reaches 0.098Mpa, the temperature is slowly raised to intercept the mixture of phenylphosphonium dichloride and phenylphosphonic dichloride. After the high boiler is cooled, put in 50g of toluene, wash with saturated sodium carbonate to neutrality, wash the organic layer twice with deionized water, separate the organic layer, distill to recover the toluene, put 30g of ethanol in the bottle, and recrystallize to obtain three Phenylphosphine was 21.6g, the yield was 82.4%, and the content detected by HPLC was 98.5%.

Embodiment 3

[0047] Put 27.8g of triphenylphosphine oxide, 88.2g of diphenylphosphine chloride (the mass ratio of the two is 1:3.17), and 0.56g of diphenylphosphonic acid (triphenylphosphine oxide) into the 250mL reaction flask replaced by nitrogen. 2% of the mass), the temperature is raised to 150°C, and the temperature is kept for 12h. After cooling to room temperature, turn on the vacuum pump. After the vacuum degree reaches 0.098Mpa, the temperature is slowly raised to intercept the mixture of diphenylphosphine chloride and diphenylphosphinyl chloride. After the high boiler is cooled, put in 50g of toluene, wash with saturated sodium carbonate to neutrality, wash the organic layer twice with deionized water, separate the organic layer, distill to recover the toluene, put 30g of ethanol in the bottle, and recrystallize to obtain three Phenylphosphine 18.4g, the yield was 70%, and the content detected by HPLC was 97.8%.

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Abstract

The invention provides a method for preparing triphenylphosphine in a reducing manner. Phenylphosphonicdichloride or chlorodiphenylphosphine is used as a reducing agent, and raw materials are low in price and easily obtained; under the effect of a catalyst, the phenylphosphonicdichloride or chlorodiphenylphosphine and triphenylphosphine oxide are subjected to reducing reaction, stabilities of phosphine oxygen double bonds in the triphenylphosphine oxide and oxidation products (phenylphosphonic dichloride or diphenylphosphinyl chloride) of a reducing agent are different, the stabilities of thedouble bonds of the phenylphosphonic dichloride and the diphenylphosphinyl chloride are good, the double bonds of the triphenylphosphine oxide are broken under the effect of the catalyst, the double bonds of the formed phenylphosphonic dichloride and the formed diphenylphosphinyl chloride are not easily damaged by the catalyst, and therefore, triphenylphosphine can be obtained under gentle conditions; the oxidation products (the phenylphosphonic dichloride or the diphenylphosphinyl chloride) of the reducing agent are important organic synthesis intermediate (such as synthesis of organic phosphate); and moreover, the amount of the catalyst required in the method is small, and the catalysis efficiency is high.

Description

Technical field [0001] The present invention relates to the technical field of compound preparation, in particular to a method for reducing and preparing triphenylphosphine. Background technique [0002] Organic phosphine compounds and their derivatives have a wide range of applications in the fields of life sciences and chemical engineering, especially triphenylphosphine, which plays an important role in organometallic catalysis and many classical organic reactions, such as witting reaction, Appel Response etc. However, the reaction is often accompanied by the formation of triphenylphosphine oxide as a by-product. Therefore, how to eliminate by-products or realize the effective utilization of useless by-products has attracted more and more attention. Among them, reducing triphenylphosphine oxide to triphenylphosphine is an effective method to increase the added value of the reaction. [0003] At present, the reduction methods of triphenyl phosphine oxide mainly include: (1) Phos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/50
CPCC07F9/5022C07F9/509
Inventor 段好东张召举李焕成王祥王忠卫
Owner 江苏富比亚化学品有限公司
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