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Synthetic process of rhodium caprylate dimer

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

Active Publication Date: 2009-01-28
浙江微通催化新材料有限公司
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Problems solved by technology

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

Method used

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Embodiment 1

[0014] Example 1: The present invention mainly adopts the following two procedures. The first step is to add 26.2g of rhodium trichloride trihydrate to 400ml of DMF (N,N-dimethylformamide) and 42.0g of dimethylamine acetate. In 400ml acetic acid, 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 filter; add the resulting filter cake to 400ml methanol After refluxing for 3 hours, it was cooled to zero and filtered. The filter cake was directly added to 400ml of toluene and refluxed for 2 hours. Then it was changed to a distillation device, and half of the volume was distilled and cooled. Filtration, vacuum drying, to obtain 16.1 g of rhodium acetate dimer product, the product purity is above 99%, and the yield is 72.8%;

[0015] The elemental analysis results of the obtained rhodium acetate are as follows: C, 21.93%; H, 2.85%; N: 0%...

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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 invention relates to an improvement in the synthesis circuit and process of rhodium octanoate dimer, which is an important catalyst in basic chemical industry and pharmaceutical chemical industry, and related intermediate raw material rhodium acetate dimer. technical background [0002] As a homogeneous catalyst, rhodium octoate has outstanding performance in cyclopropanation, hydroformylation, Cl chemistry such as carbonylation and ethylene glycol process, cycloisomerization, etc., especially in cyclopropanation. Rhodium catalyst is other Metal is irreplaceable. At the same time, rhodium octanoate 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 cyproboronic acid, ciprofloxacin, etc. On electron-deficient olefins and heterocyclic olefins, onl...

Claims

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Application Information

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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
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