Synthesis method for preparing triphenylphosphine through reduction of triphenylphosphine oxide

Abstract

The invention relates to a synthesis method for preparing triphenylphosphine through reduction of triphenylphosphine oxide, and belongs to the technical field of organic synthesis.The preparation method comprises the following steps that 1, a methanol solvent and triphenylphosphine oxide are added into a pressure kettle, magnesium chips are added, the molar ratio of triphenylphosphine oxide to magnesium chips is 1.0: 1.0-1.5, the reaction temperature is controlled to range from 90 DEG C to 100 DEG C, and the heat preservation time ranges from 2 hours to 3 hours; and Step 2, after the reaction is finished, cooling to room temperature, filtering, concentrating filtrate, and recovering the solvent to obtain the triphenylphosphine. According to the invention, triphenylphosphine oxide is used as a raw material, and is reduced by magnesium chips in a solvent to obtain triphenylphosphine. Compared with a traditional reduction synthesis method, silane or diisobutylaluminium hydride which is high in process risk and flammable and explosive does not need to be used, so that the safety of the synthesis process can be effectively improved, expensive reagents and electrode materials do not need to be used, the raw materials used in the synthesis method are cheap and easy to obtain, the process is green, safe and efficient, the yield is high, and the method is suitable for industrial production. The method is suitable for industrial large-scale production.

Description

Technical Field

[0001] The present invention relates to the technical field of organic synthesis, and particularly to a synthetic method for preparing triphenylphosphine by reducing triphenylphosphine oxide. Background Art

[0002] Triphenylphosphine has a wide range of uses in the field of fine chemicals. It is an important catalyst ligand in contemporary petrochemical and fine chemical production, and can also be used in new materials for catalyst carriers, etc. It can also be used as a promoter, flame retardant, heat stabilizer, antistatic agent, etc. Triphenylphosphine has great economic and social benefits, and it is very necessary to develop, produce and optimize its synthetic process.

[0003] Currently, the main synthetic methods for preparing triphenylphosphine by reducing triphenylphosphine oxide are: reducing with silane or diisobutylaluminum hydride as the reducing agent. This reduction method has high prices for raw materials such as silane or diisobutylaluminum hydride, and the synthetic process is highly dangerous. There is also the use of electrochemical reduction method for reduction. This method has expensive electrode materials and low yields, and is not suitable for industrial production.

[0004] Therefore, seeking a synthetic method for preparing triphenylphosphine by reducing triphenylphosphine oxide that is economical, environmentally friendly, and has a safe and efficient process is still a research hotspot in this field. Summary of the Invention

[0005] The present invention provides a synthetic method for preparing triphenylphosphine by reducing triphenylphosphine oxide, which solves the problems raised in the above background art. This reduction synthesis method uses triphenylphosphine oxide as the raw material and obtains triphenylphosphine by reduction with magnesium chips in a solvent. It has the characteristics of simple process, safe and green, and low raw material cost, and is suitable for industrial production.

[0006] The solution of the present invention to the above technical problems is as follows: A synthetic method for preparing triphenylphosphine by reducing triphenylphosphine oxide, and its preparation method includes the following:

[0007] Step1: Add methanol solvent and triphenylphosphine oxide into an autoclave, add magnesium chips, and the molar ratio of triphenylphosphine oxide to magnesium chips is 1.0:1.0 - 1.5. Control the reaction temperature at 90 - 100 °C, and keep the temperature for 2 - 3 hours;

[0008] Step2: After the reaction ends, filter, and the filtrate is concentrated to recover the solvent to obtain triphenylphosphine. The synthetic process route is as follows:

[0009]

[0010] Based on the above technical solution, the present invention can also be improved as follows.

[0011] Further, the methanol solvent can be replaced with a single solvent or a mixed solvent of alcohols such as methanol and ethanol.

[0012] The beneficial effects of the present invention are as follows: The present invention provides a synthesis method for the reduction of triphenylphosphine oxide to prepare triphenylphosphine, which has the following advantages:

[0013] 1. Using triphenylphosphine oxide as the raw material, triphenylphosphine is obtained by reduction with magnesium chips in a solvent. Compared with the traditional reduction synthesis method, there is no need to use silane or diisobutylaluminum hydride, which are highly flammable, explosive and have high process hazards, thus effectively improving the safety of the synthesis process;

[0014] 2. There is no need to use expensive reagents and electrode materials. The raw materials used in this synthesis method are cheap and easily available. The process is green, safe, efficient, has a high yield, and is suitable for industrial scale-up production.

[0015] The above description is only an overview of the technical solution of the present invention. In order to be able to understand the technical means of the present invention more clearly and implement it in accordance with the content of the specification, the following provides a detailed description of the preferred embodiments of the present invention. The specific implementation manners of the present invention are given in detail by the following embodiments. Specific implementation manners

[0016] The principles and features of the present invention are described below. The examples given are only used to explain the present invention and are not intended to limit the scope of the present invention. The present invention is described more specifically by way of example in the following paragraphs. The advantages and features of the present invention will be clearer according to the following description and claims.

[0017] It should be noted that when a component is referred to as being "fixed to" another component, it can be directly on the other component or there can also be an intermediate component. When a component is considered to be "connected" to another component, it can be directly connected to the other component or there may be an intermediate component at the same time. When a component is considered to be "disposed on" another component, it can be directly disposed on the other component or there may be an intermediate component at the same time. The terms "vertical", "horizontal", "left", "right" and similar expressions used herein are only for the purpose of illustration.

[0018] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field to which the present invention belongs. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0019] The present invention provides a synthesis method for the reduction of triphenylphosphine oxide to prepare triphenylphosphine, and its method flow includes the following:

[0020] Step 1: Add 100.0 g of methanol and triphenylphosphine oxide (27.8 g, 0.1 mol) into an autoclave, add 2.6 g of magnesium chips, and heat to 90 - 100 °C for heat preservation reaction for 3 hours;

[0021] Step 2: After the reaction is completed, cool to room temperature, filter, and concentrate the filtrate to recover the solvent to obtain 26.2 g of triphenylphosphine, with a yield of 99% and a purity of 99%.

[0022] 1 H NMR (400 MHz, CDCl3) δ 7.24 - 7.34 (15H);

[0023] As described above, it is only the preferred embodiment of the present invention and does not impose any formal restrictions on the present invention; any ordinary technical personnel in this industry can smoothly implement the present invention according to the above description; however, any equivalent changes such as slight modifications, evolutions made by those skilled in this professional field without departing from the technical solution of the present invention by using the technical content disclosed above are all equivalent embodiments of the present invention; at the same time, any equivalent changes, modifications, and evolutions made to the above embodiments based on the essential technology of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims

1. A synthetic method for preparing triphenylphosphine by reducing triphenylphosphine oxide, wherein the preparation method comprises the following steps: Step 1: Add methanol solvent and triphenylphosphine oxide into the autoclave, add magnesium chips, the molar ratio of triphenylphosphine oxide to magnesium chips is 1.0:1.0-1.5, control the reaction temperature to 90-100°C, and keep warm for 2-3 hours; Step 2: After the reaction is completed, the mixture is cooled to room temperature, filtered, and the filtrate is concentrated and the solvent is recovered to obtain triphenylphosphine. The synthesis process route is as follows:

2. A method for preparing triphenylphosphine by reducing triphenylphosphine oxide according to claim 1, characterized in that: The methanol solvent can be replaced by a single solvent or a mixed solvent of alcohols such as methanol and ethanol.

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