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Preparation method of rhodium octoate dimer

A technology of rhodium octanoate dimer and octanoic acid, which is applied in the field of preparation of rhodium octanoate dimer, can solve the problems of high yield of target product, complicated operation, expensive raw materials, etc., and achieves easy-to-obtain raw materials, simple operation, and improved yield Effect

Active Publication Date: 2020-09-29
SHANGHAI WOKAI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the defects of low yield, complicated operation and expensive raw materials in the prior art rhodium octanoate dimer preparation method, the present invention provides a kind of octanoic acid The preparation method of the rhodium dimer utilizes a two-step method, first carries out ligand replacement with RhCl3 and octanoic acid alkali metal salt, obtains the intermediate product rhodium octanoate (Ⅲ), and then passes the weak reducing agent to The reduction of octanoic acid rhodium (III) to octanoic acid rhodium (II) is simple, the raw materials are easily available, and the yield of the target product obtained is high

Method used

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  • Preparation method of rhodium octoate dimer

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Effect test

Embodiment 1

[0028] A kind of preparation method of rhodium octanoate dimer, comprises the steps:

[0029] (1) In a 500ml single-necked flask, add 5.3g (25.3mmol) RhCl 3 Mix well with 12.3g (74mmol) sodium caprylate (octanoic acid alkali metal salt), obtain the first solution;

[0030] (2) Add 200 mL of ethanol (reducing agent) to the first solution in step (1), and heat to 80° C. for reflux reaction for 4 hours to obtain a dark green second solution;

[0031] (3) Under the condition of stirring, slowly add the second solution obtained in step (2) into 800mL deionized water while hot, and a large amount of dark green solid precipitates out immediately. After the addition, continue to stir for 1h and suction filter to obtain the crude product green solid;

[0032] (4) Suspend the crude product obtained in step (3) in 400mL 10wt% NaHCO 3 Stir in the aqueous solution for 1 hour, wash thoroughly to remove the water-soluble by-products NaCl and sodium octanoate (one wash), and collect the so...

Embodiment 2

[0034] A kind of preparation method of rhodium octanoate dimer, comprises the steps:

[0035] (1) In a 500ml single-necked flask, add 4.4g (21.2mmol) RhCl 3 Mix well with 12.3g (74mmol) sodium caprylate (octanoic acid alkali metal salt), obtain the first solution;

[0036] (2) Add 100 mL of n-butanol (reducing agent) to the first solution in step (1), and heat to 70° C. for reflux reaction for 8 hours to obtain a dark green second solution;

[0037] (3) Under the condition of stirring, slowly add the second solution obtained in step (2) into 800mL deionized water while hot, and a large amount of dark green solid precipitates out immediately. After the addition, continue to stir for 1h and suction filter to obtain the crude product green solid;

[0038] (4) Suspend the crude product obtained in step (3) in 400mL 10wt% NaHCO 3 Stir in the aqueous solution for 1 hour, wash thoroughly to remove the water-soluble by-products NaCl and sodium octanoate (one wash), and collect the ...

Embodiment 3

[0040] A kind of preparation method of rhodium octanoate dimer, comprises the steps:

[0041] (1) In a 500ml single-necked flask, add 5.3g (25.3mmol) RhCl 3 Mix well with 18.9g (113.7mmol) sodium caprylate (octanoic acid alkali metal salt), obtain the first solution;

[0042](2) Add 300 mL of isopropanol (reducing agent) to the first solution in step (1), and heat to 80° C. for reflux reaction for 12 hours to obtain a dark green second solution;

[0043] (3) Under the condition of stirring, slowly add the second solution obtained in step (2) into 800mL deionized water while hot, and a large amount of dark green solid precipitates out immediately. After the addition, continue to stir for 1h and suction filter to obtain the crude product green solid;

[0044] (4) Suspend the crude product obtained in step (3) in 400mL 10wt% NaHCO 3 Stir in the aqueous solution for 1 hour, wash thoroughly to remove the water-soluble by-products NaCl and sodium octanoate (one wash), and collect...

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Abstract

The invention belongs to the technical field of homogeneous catalyst preparation, and particularly relates to a preparation method of a rhodium octoate dimer. The preparation method comprises the following steps: (1) uniformly mixing RhCl3 and an alkali metal octoate to obtain a first solution; (2) adding a reducing agent into the first solution in step (1), and heating for a reflux reaction to obtain a second solution; (3) adding the second solution obtained in step (2) into deionized water while the second solution is hot, continuously stirring, and carrying out suction filtration to obtaina crude product; and (4) carrying out primary washing, secondary washing, filtering and drying on the crude product obtained in step (3) to obtain the green solid rhodium octoate dimer. The method issimple to operate, raw materials are easy to obtain, the obtained target product is high in purity (98% or above) and high in yield (the total yield is 80% or above), and the requirements of industrial production can be met.

Description

technical field [0001] The invention belongs to the technical field of preparation of homogeneous catalysts, in particular to a preparation method of rhodium octanoate dimer. Background technique [0002] Transition metal catalysts (such as rhodium, palladium, ruthenium, etc.) realize the conversion from linear compounds to cyclic compounds. The structure of rhodium(II) octanoate is similar to that of rhodium(II) acetate, with a double nucleic acid bridge lantern structure. As a homogeneous catalyst, rhodium octanoate dimer has remarkable catalytic activity for C-H insertion reaction, and is an important catalyst for pharmaceutical and chemical industries. The catalytic effect is outstanding in reactions such as cyclopropanation and hydroformylation. Diazoamide generates β-lactams under the catalysis of Rh(II), and this has become an important way to synthesize β-lactams. Rhodium n-octanoate is just a key catalyst in the synthesis of such products. Giround-Godgium et al f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C53/126
CPCC07C51/418C07C53/126
Inventor 秦建国王聪孙鑫周文辉
Owner SHANGHAI WOKAI BIOTECH