Microwave synthetic method of tri(triphenylphosphine) rhodium chloride

A technology of rhodium trichloride trihydrate and triphenylphosphine, which is applied in the field of microwave synthesis of rhodium trichloride, can solve problems such as complex process routes, and achieve the effects of simplified process flow, high purity, and high yield

Active Publication Date: 2009-01-28
浙江微通催化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Netherlands patent NL6602062A has reported the preparation of a series of organophosphine ligand rhodium chloride compounds, and German patent DE10200572A1 has reported that three (triphenylphosphine) rhodium chlorides have been synthesized by raising the temperature step by step, all of which have problems such as too complicated process routes

Method used

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  • Microwave synthetic method of tri(triphenylphosphine) rhodium chloride
  • Microwave synthetic method of tri(triphenylphosphine) rhodium chloride
  • Microwave synthetic method of tri(triphenylphosphine) rhodium chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0019] In a 1L flask equipped with a mechanical stirrer and a reflux condenser, dissolve 10.0g of rhodium trichloride trihydrate in 200ml of 90% ethanol; add 500ml of ethanol solution containing 60g of pretreated triphenylphosphine, place in microwave In the reactor, react under 700W power microwave radiation for 5 minutes to form a large number of dark red crystals; cool to 40°C, filter the product obtained by suction, wash it with 100ml of anhydrous ether, and dry it in vacuum at 50°C for 2 hours to obtain dark red crystals Product, yield 34.7g, yield 98.8%; Elemental analysis: C: 70.30%; H: 5.13%; N: 0%, Rh element content measured by atomic absorption is 11.0%.

Embodiment 2

[0021] The reaction steps are the same as in Example 1, except that the microwave radiation power is 400W, and the reaction time is 20 minutes. The post-treatment operation is the same as in Example 1, and the product yield is 98.4%.

Embodiment 3

[0023] The reaction steps are the same as in Example 1, except that the nitrogen protection is applied, and the reaction time is 5 minutes. The post-treatment operation is the same as in Example 1, and the product yield is 99.0%.

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Abstract

The invention relates to a method for synthesizing rhodium chloride (triphenylphosphine). The method of the invention takes rhodium chloride trihydrate and triphenylphosphine with the mass ratio of 1:5 to 5 as main raw materials for synthesizing the rhodium chloride (triphenylphosphine) rhodium in an alcohol-water mixed solvent under the condition of microwave radiation, wherein, the microwave radiation power ranges from 100 to 1000W, microwave reaction time lasts for 5 to 30 minutes, and the reaction formula is as the formula. The method has the advantages of high heating speed, short reaction time, high reaction yield, simple and convenient reaction operation, simple treatment after reaction and simplified process flow, etc.

Description

technical field [0001] The invention relates to a microwave synthesis method of tris(triphenylphosphine) rhodium chloride. Background technique [0002] Tris(triphenylphosphine) rhodium chloride is the first coordination compound used as a hydrogenation catalyst in a homogeneous solution discovered in 1965 by the Nobel Laureate in Chemistry, G.Wilkinson of the United Kingdom. As a hydrogenation catalyst for unsaturated organic molecules, it can carry out reactions such as catalytic hydrogenation, aldehyde decarbonylation, and partial substitution of propylene under mild conditions, and is widely used in olefin selective hydrogenation, carbonylation, and formylation reactions. [0003] The traditional process of synthesizing three (triphenylphosphine) rhodium chloride was reported by Osborn, J., etc. in 1967 (Inorg, Synth.10, 67), but there are large solvent consumption and low yields. Dutch patent NL6602062A reports the preparation of a series of organophosphine ligand rhod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C07F9/50B01J31/24B01J31/30
Inventor 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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