Method for preparing bis(norbornadiene)rhodium tetrafluoroborate

A technology of rhodium tetrafluoroborate and norbornanol, which is applied in chemical instruments and methods, purification/separation of hydrocarbons, organic chemistry, etc., can solve the problems of high preparation cost, cumbersome process, low yield, etc., and achieve improved yield and Purity, simple preparation method, and the effect of reducing production costs

Active Publication Date: 2020-05-01
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Bis(norbornadiene) rhodium tetrafluoroborate has unstable physical and chemical properties and is prone to react with oxygen. The existing preparation method has complex processes, low yield and high preparation cost, which is unfavorable for popularization and use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for preparing two (norbornadiene) rhodium tetrafluoroborates, comprising the following steps:

[0024] (1) Take rhodium trichloride hydrate and norbornadiene at a ratio of 1:3.0, put them in a pre-deoxidized methanol solvent, heat to reflux, the reflux temperature is 75°C, and the reflux time is For 3h, after concentrating and filtering, obtain norbornadiene rhodium chloride dimer;

[0025] (2) In a nitrogen-protected environment, dissolve the norbornadiene rhodium chloride dimer obtained in step (1) in a pre-deoxygenated dichloromethane solvent, and then add silver tetrafluoroborate to carry out ion exchange reaction , the reaction times is 10h, obtains two (norbornadiene) rhodium tetrafluoroborate solutions;

[0026] Wherein, the ratio of the substance amount of norbornadiene rhodium chloride dimer and silver tetrafluoroborate is 1:2.5;

[0027] (3) In a nitrogen-protected environment, in the bis(norbornadiene)rhodium tetrafluoroborate solution described in...

Embodiment 2

[0029] A method for preparing two (norbornadiene) rhodium tetrafluoroborates, comprising the following steps:

[0030] (1) Take rhodium trichloride hydrate and norbornadiene according to the ratio of 1:6.0, put them in the ethanol solvent that has been deoxidized beforehand, heat to reflux, the reflux temperature is 85°C, and the reflux time is For 1h, after concentrating and filtering, obtain norbornadiene rhodium chloride dimer;

[0031] (2) Under the protection of argon, dissolve the norbornadiene rhodium chloride dimer obtained in step (1) in the pre-deoxygenated 1,2-dichloroethane solvent, and then add tetrafluoroboric acid Silver, carries out ion exchange reaction, and the reaction times is 18h, obtains two (norbornadiene) rhodium tetrafluoroborate solutions;

[0032] Wherein, the ratio of the substance amount of norbornadiene rhodium chloride dimer to silver tetrafluoroborate is 1:3.0;

[0033] (3) In an argon-protected environment, add tetrahydrofuran to the bis(norb...

Embodiment 3

[0035] A method for preparing two (norbornadiene) rhodium tetrafluoroborates, comprising the following steps:

[0036] (1) Take rhodium trichloride hydrate and norbornadiene at a ratio of 1:5.0, put them in ethanol solvent that has been pre-deoxidized, and heat to reflux. The reflux temperature is 80°C, and the reflux time is For 2h, after concentrating and filtering, obtain norbornadiene rhodium chloride dimer;

[0037] (2) Under an argon-protected environment, dissolve the norbornadiene rhodium chloride dimer obtained in step (1) in a pre-deoxidized chloroform solvent, and then add silver tetrafluoroborate to carry out ion exchange reaction, The reaction time was 15h, and two (norbornadiene) rhodium tetrafluoroborate solutions were obtained;

[0038] Wherein, the ratio of the substance amount of norbornadiene rhodium chloride dimer to silver tetrafluoroborate is 1:3.5;

[0039] (3) In an argon-protected environment, in the bis(norbornadiene)rhodium tetrafluoroborate soluti...

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PUM

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Abstract

The invention belongs to the technical field of precious metal preparation, and relates to a method for preparing bis(norbornadiene)rhodium tetrafluoroborate. A red bis(norbornadiene)rhodium tetrafluoroborate solid is obtained by subjecting rhodium trichloride hydrate and norbornadiene serving as raw materials to an ion exchange reaction with silver tetrafluoroborate in an inert gas protection environment and carrying out filter pressing. The preparation method is simple, the yield and the purity of a bis(norbornadiene)rhodium product are improved, and production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of precious metal preparation, and relates to the synthesis of a rhodium complex, in particular to a method for preparing bis(norbornadiene) rhodium tetrafluoroborate. Background technique [0002] Metal rhodium complexes are widely used in organometallic chemistry and organic synthetic chemistry. Bis(norbornadiene) rhodium tetrafluoroborate is not only a raw material for the synthesis of many complex metal rhodium complexes, but also often used together with other ligands to jointly catalyze the occurrence of many reactions such as coupling, hydrogenation and addition. [0003] Bis(norbornadiene) rhodium tetrafluoroborate is unstable in physical and chemical properties, and is easy to react with oxygen. The existing preparation method has cumbersome process, low yield and high preparation cost, which is not conducive to popularization and use. Contents of the invention [0004] For above-mentioned prior ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/38C07C7/00C07C13/42
CPCC07C2/38C07C7/005C07C2602/42C07C13/42
Inventor 张高鹏潘丽娟朱大川韩彬
Owner XIAN CATALYST NEW MATERIALS CO LTD
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