A kind of preparation method of 1,5-cyclooctadiene iridium chloride dimer

A technology of cyclooctadiene iridium chloride and cyclooctadiene is applied in the field of preparation of 1,5-cyclooctadiene iridium chloride dimer, which can solve the problem of high purity and yield of dimer, and high reaction time. It can reduce the production cost, reduce the loss of waste liquid treatment, and reduce the amount of use.

Active Publication Date: 2019-05-03
NUTRICHEM LAB CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the ubiquitous 1,5-cyclooctadiene and water consumption in the existing 1,5-cyclooctadiene iridium chloride dimer preparation method, long reaction time, product purity and The defect of low yield provides a kind of preparation method of 1,5-cyclooctadiene iridium chloride dimer, and this method 1,5-cyclooctadiene and water consumption are few, and reaction time is short, 1,5 - High purity and yield of cyclooctadiene iridium chloride dimer

Method used

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  • A kind of preparation method of 1,5-cyclooctadiene iridium chloride dimer
  • A kind of preparation method of 1,5-cyclooctadiene iridium chloride dimer
  • A kind of preparation method of 1,5-cyclooctadiene iridium chloride dimer

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preparation example Construction

[0018] The invention provides a method for preparing 1,5-cyclooctadiene iridium chloride dimer. The method comprises: under anaerobic conditions, iridium-containing chlorine-containing compounds, aldehydes, 1,5-cyclooctadiene React with solvents.

[0019] According to the method of the present invention, the oxygen-free condition can be ensured by introducing an inert gas replacement into the reactor, and the number of replacements is not particularly limited, preferably 3-5 times, and the inert gas can be nitrogen, argon, At least one of helium and neon, preferably argon.

[0020] According to the present invention, preferably, the weight ratio of the iridium-containing chlorine-containing compound to the solvent is 1:5-20, and more preferably, the weight ratio of the iridium-containing chlorine-containing compound to the solvent is 1:5-10. In the preparation method of 1,5-cyclooctadiene iridium chloride dimer provided by the prior art, the amount of solvent used is large, a...

Embodiment approach

[0027] According to a preferred embodiment of the present invention, the method further includes: cooling, washing, filtering and drying in sequence after the contact reaction. The cooling, filtering, washing and drying can all be carried out according to conventional means in the art.

[0028] According to the present invention, preferably, the cooling is to naturally cool down to room temperature, and then transfer to an ice-water bath. Adopting this preferred embodiment is more conducive to the precipitation of products.

[0029] In the present invention, the filtration may be suction filtration.

[0030] In the present invention, the washing may be to sequentially use water and cold methanol to wash the filter cake obtained by suction filtration.

[0031] The present invention has no special limitation on the drying, and the drying can be carried out at room temperature under vacuum.

[0032] The present invention has no particular limitation on the embodiment of the con...

Embodiment 1

[0040] This example is used to illustrate the preparation method of the 1,5-cyclooctadiene iridium chloride dimer provided by the present invention.

[0041] At room temperature (25°C), add 1 g of iridium trichloride monohydrate (3.1 mmol) with a mass content of 98% and 5 g of deoxygenated water (obtained by bubbling argon for 10 min) into a reaction flask filled with argon, and depressurize Replace argon 3 times, heat up to 80°C, add 1.38g of 40% acetaldehyde aqueous solution (acetaldehyde 12.5mmol), 1.4g of 98% 1,5-cyclooctadiene (12.7mmol) , reflux at 80°C for 6h, cool the reaction mixture to room temperature, transfer to an ice-water bath (0°C) for 1h, then perform suction filtration (2°C), wash with water (1g water, 1g cold methanol rinse) And drying (room temperature 25° C., 6 h), a red solid 0.77 g was obtained. The measured yield was 74%. The red solid is analyzed and determined by proton nuclear magnetic resonance spectroscopy, and the melting point of the red solid...

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Abstract

The invention relates to the field of noble metal catalyst synthesis, and discloses a method for preparing chloro(1,5-cyclooctadiene)iridium(I) dimer. The method includes the step that under the oxygen-free condition, an iridium-containing and chlorine-containing compound, aldehyde, 1,5-cyclooctadiene and solvent are subjected to a contact reaction. Traditionally used reactants (alcohol) are abandoned, and new reactants (aldehyde) are used, so the yield of chloro(1,5-cyclooctadiene)iridium(I) dimer can be as high as 75% in short reaction time. Consumption of water and 1,5-cyclooctadiene is low, waste liquid treatment loss is greatly reduced, and production cost is reduced.

Description

technical field [0001] The invention relates to the field of noble metal catalyst synthesis, in particular to a preparation method of 1,5-cyclooctadiene iridium chloride dimer. Background technique [0002] Asymmetric catalytic hydrogenation is a hotspot in the field of organic synthetic chemistry research. Researchers have developed a variety of chiral ruthenium and rhodium complex catalysts, which have achieved good catalytic effects in the process of asymmetric catalytic hydrogenation reactions. However, due to the specificity of the catalytic hydrogenation reaction, each catalyst is only effective for one or a few types of specific substrates. In addition, chiral catalysts also have disadvantages such as high dosage, harsh conditions, and long reaction time. [0003] In addition to ruthenium and rhodium complex catalysts, complexes formed by transition metal iridium and chiral ligands are also widely used in asymmetric catalytic hydrogenation reactions, especially for t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02B01J31/22
CPCB01J31/2295B01J2531/827C07F17/02
Inventor 汪春华陈笑宇蔡玉梅
Owner NUTRICHEM LAB CO LTD
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