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Metal rhodium-1,2-di(diphenyl phosphine)ethane complex crystal and preparation method thereof

A technology of diphenylphosphine and complexes, which is applied in the field of metal rhodium-1,2-bisethane complex crystals and its preparation, which can solve the problems of cumbersome process and achieve the effect of simple and easy preparation method and mild conditions

Inactive Publication Date: 2014-07-30
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process is more cumbersome

Method used

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  • Metal rhodium-1,2-di(diphenyl phosphine)ethane complex crystal and preparation method thereof
  • Metal rhodium-1,2-di(diphenyl phosphine)ethane complex crystal and preparation method thereof

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preparation example Construction

[0021] The preparation method of metallic rhodium-1,2-bis(diphenylphosphine)ethane complex crystal comprises the following steps:

[0022] 1) Prepare 0.8-1.2g / L rhodium chloride aqueous solution, then add stannous chloride to it, place the solution in a 45-55°C water bath for 40-60min, and then place it at room temperature to cool;

[0023] 2) Add 1,2-bis(diphenylphosphine)ethane tetrahydrofuran solution to the above system to obtain light yellow precipitate; the 1,2-bis(diphenylphosphine)ethane tetrahydrofuran solution The concentration is 0.08-0.12g / L;

[0024] 3) Add dichloromethane to the above system to form layers, then volatilize the solvent and generate products at the phase interface.

[0025] The volume ratio of the rhodium chloride aqueous solution in step 1) to the tetrahydrofuran solution of 1,2-bis(diphenylphosphine)ethane in step 2) is 1:(0.8-1.2).

[0026] In step 1), the molar ratio of stannous chloride to rhodium chloride is 3.5-4.5:1.

[0027] The volume ...

Embodiment 1

[0030] Prepare 5ml of 1g / L rhodium chloride solution, add stannous chloride at a molar ratio of 4:1 (the molar ratio of stannous chloride to rhodium chloride is 4:1), put it in a water bath at 50°C for 1 hour, and the solution changes from The dark yellow turns into deep purple, and then left to cool at room temperature. Add 5ml of tetrahydrofuran solution of 1,2-bis(diphenylphosphine)ethane with a concentration of 0.1g / L to form a pale yellow precipitate;

[0031] Add 5ml of dichloromethane to the above system, layered into two phases, let the solvent evaporate until the volume of the system is 10ml, it can be seen that crystals are generated between the layered two phases.

Embodiment 2

[0033] Take out the crystal, carry out corresponding crystal structure analysis, the result is as follows:

[0034] Table 1:

[0035]

[0036] figure 1 It is the molecular structure and atomic label of the crystal obtained in the present invention.

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Abstract

The invention discloses a metal rhodium-1,2-di(diphenyl phosphine)ethane complex crystal, which belongs to a monoclinic system, the space group is P21 / c, and the cell parameters are a(A) is 11.5646(8), b(A) is 14.1442(10), and c(A) is 17.2350(12). The preparation method of the metal rhodium-1,2-di(diphenyl phosphine)ethane complex crystal comprises the following steps: 1)preparing a 0.8-1.2g / L of rhodium chloride aqueous solution, adding stannous chloride, placing the solution under the temperature of 45-55 DEG C and keeping the setting time, placing the solution under room temperature and then cooling; 2)adding a 1,2-di (diphenylphosphine)ethane tetrahydrofuran solution in the above system to obtain the light yellow deposition; wherein the concentration of the solution is 0.08-0.12g / L; and 3)adding dichloromethane in the above system for layering, then volatilizing the solution, and generating the products at phase interface. The preparation method has the advantages of easy operation and mild condition, a traditional method for adopting a heating backflow mode is not used, and a new compound with latent catalysis performance is finally obtained.

Description

technical field [0001] The invention relates to metal rhodium-1,2-bis(diphenylphosphine)ethane complex crystal and a preparation method thereof. Background technique [0002] Rhodium compounds, as noble metal homogeneous catalysts, have been widely used in important chemical processes such as hydroformylation, hydrogenation, and oxo synthesis. In the mid-1950s, it was found that rhodium complexes had higher activity for hydroformylation than cobalt, which allowed the reaction to be carried out under milder operating conditions (lower temperature and pressure). At present, triphenylphosphine rhodium chloride is a well-developed catalyst. Many researchers have done a lot of research on its physical and chemical properties and catalytic performance, showing that the triphenylphosphine rhodium chloride catalyst containing a phosphine bridge structure is active. High selectivity, mild operating conditions, and effective reduction of double and triple bonds. Therefore, the resear...

Claims

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Application Information

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IPC IPC(8): C07F19/00
Inventor 李耀威刘健曾荣华
Owner SOUTH CHINA NORMAL UNIVERSITY
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