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Synthetic process of rhodium caprylate dimer

A technology of rhodium octanoate dimer and rhodium acetate dimer is applied in the field of synthesis technology of rhodium octanoate dimer, can solve the problems of complicated processing, low final yield, long reaction time, etc. high yield effect

Active Publication Date: 2011-04-20
浙江微通催化新材料有限公司
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Malcolm H.Chi sholm, etc. published an article on Inorg.Chem in 1996 and reported the synthetic method of octanoic acid rhodium, wherein the reaction time is too long, it needs several consecutive days, the post-processing is complicated, and the final yield is also low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: the present invention mainly adopts following two procedures, the first step: 26.2g rhodium trichloride trihydrate is joined in 400ml DMF (N, N-dimethylformamide), and 42.0g dimethylamine acetate is added Add the rhodium trichloride solution to the acetic acid solution under reflux conditions and reflux for 4 hours, cool to zero and filter, wash with equal volumes of glacial acetic acid and methanol, and then filter; add the resulting filter cake to 400ml of methanol After 3 hours of reflux, cool to zero and filter. The filter cake is directly added to 400ml of toluene and refluxed for 2 hours. After reflux for 2 hours, it is changed to a distillation device, and half of the volume is distilled off and then cooled. Filtration, vacuum drying, obtain rhodium acetate dimer product 16.1g, product purity more than 99%, yield 72.8%;

[0015] The obtained rhodium acetate element analysis results are as follows: C, 21.93%; H, 2.85%; N: 0%. Rh content measured by ...

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Abstract

A synthetic process of a rhodium octanoate dimer comprises the following two steps: firstly, a DMF solvent of rhodium chloride is added to acetate solution of acetate dimethylamine to generate (Me2NH2]2[Rh2(CH3COO)4Cl2) which is heated in hot water to prepare (Rh2(CH3COO)4).2H2O; then the (Rh2(CH3COO)4).2H2O is dissolved in hot toluene to obtain the rhodium acetate dimer; secondly, the rhodium octanoate dimer is synthesized by a soxhlet extractor. By adopting the method of exchanging and separating the octanoic acid and the acetate dimmer at the same time, chlorobenzene backflow is utilized to keep the system at constant temperature to obtain a pure product of the rhodium octanoate dimer. The synthetic process is characterized by high reaction yield, high product purity, less loss of precious metals, etc.

Description

technical field [0001] The present invention relates to the improvement of the synthesis circuit and process of the important catalyst rhodium octanoate dimer and the related intermediate raw material rhodium acetate dimer in basic chemical industry and pharmaceutical chemical industry. technical background [0002] As a homogeneous catalyst, rhodium octanoate has outstanding performance in cyclopropanation, hydroformylation, Cl chemistry such as carbonylation and ethylene glycol process, cycloisomerization, etc., especially cyclopropanation, rhodium catalysts are other Metal is irreplaceable. At the same time, rhodium octoate is also used as a precursor of many complex catalysts for the synthesis of asymmetric rhodium catalysts such as asymmetric hydroformylation. Among them, cyclopropanation can produce many medicines and pharmaceutical intermediates with cyclopropyl groups, such as ciprofloxacin, ciprofloxacin, etc. On electron-deficient olefins and heterocyclic olefins,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/126C07C51/41
Inventor 秦永年潘剑明陈波马银标魏青鞠景喜谢智平施春苗阮晓东刘斌
Owner 浙江微通催化新材料有限公司