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One-step synthesis method of (1,5-cyclooctadiene)-dichloro iridium dipolymer

A cyclooctadiene and dimer technology, applied in the field of preparation of precious metal catalysts, can solve the problems of long reaction time and harsh operation, and achieve the effects of low cost, improved yield and shortened reaction time

Inactive Publication Date: 2017-02-08
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a new synthetic method of (1,5-cyclooctadiene)-iridium dichloride dimer, which fundamentally solves the problem that the existing preparation method is relatively harsh in operation and the reaction time is too long. question

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  • One-step synthesis method of (1,5-cyclooctadiene)-dichloro iridium dipolymer

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: The preparation method of (1,5-cyclooctadiene)-iridium dichloride dimer comprises the following steps:

[0022] Weigh 2.5g (7.1 mmol) iridium trichloride hydrate, add it into a 100mL three-necked flask, repeatedly vacuumize and fill with nitrogen, and measure 50mL absolute ethanol, 0.88 mL of 1,5-cyclooctadiene (COD) was added to the reactor, and after stirring at room temperature to dissolve the solid, the reactor was transferred to an oil bath, and the reaction temperature was adjusted to 110°C, and kept The reaction temperature is heated to reflux reaction. During the reaction, the color of the solution gradually changes from dark brown to brick red. During the reaction, red crystals appear on the inner wall of the flask. After 6 hours of reaction, the reaction is stopped, cooled naturally to room temperature, and filtered under anaerobic operation. Reaction solution, then use a syringe to inject 35mL of ice-cold absolute ethanol to wash the solid in th...

Embodiment 2

[0024] Embodiment 2: the preparation method of (1,5-cyclooctadiene)-dichloroiridium dimer comprises the following steps:

[0025] Weigh 5.0g (14.2mmol) iridium trichloride hydrate, add it into a 250mL three-necked flask, repeatedly vacuumize and fill with nitrogen, and under the high-purity nitrogen atmosphere, measure 100mL of absolute ethanol, 2.11 mL of 1,5-cyclooctadiene (COD) was added to the reactor, and the solid was dissolved under stirring at room temperature, then the reactor was transferred to an oil bath, and the reaction temperature was adjusted to 120°C, and kept The reaction temperature is heated to reflux reaction. During the reaction, the color of the solution gradually changes from dark brown to brick red. During the reaction, red crystals appear on the inner wall of the flask. After 5 hours of reaction, the reaction is stopped, cooled naturally to room temperature, and filtered under anaerobic operation. Reaction solution, then use a syringe to inject 70mL o...

Embodiment 3

[0027] Embodiment 3: the preparation method of (1,5-cyclooctadiene)-iridium dichloride dimer comprises the following steps:

[0028] Take by weighing 7.5g (21.3mmol) iridium trichloride hydrate, join it in the three-necked flask of 500mL, repeatedly evacuate and fill with nitrogen, under the guarantee high-purity nitrogen atmosphere, measure successively 150mL dehydrated alcohol, 3.93 mL of 1,5-cyclooctadiene (COD) was added to the reactor, and the solid was dissolved under stirring at room temperature, then the reactor was transferred to an oil bath, and the reaction temperature was adjusted to 130°C, and kept The reaction temperature is heated to reflux reaction. During the reaction, the color of the solution gradually changes from dark brown to brick red. During the reaction, red crystals appear on the inner wall of the flask. After 4 hours of reaction, the reaction is stopped, cooled naturally to room temperature, and filtered under anaerobic operation. The reaction soluti...

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Abstract

The invention discloses a one-step synthesis method of a (1,5-cyclooctadiene)-dichloro iridium dipolymer. The method comprises the following steps: introducing nitrogen into hydrated iridous chloride; then mixing with absolute ethyl alcohol and 1,5-cyclooctadiene under a stirring condition, and carrying out a refluxing reaction, wherein a large amount of red crystals are generated on the wall of a three-necked flask after the reaction is over; after the refluxing reaction is over, naturally cooling to a room temperature, washing the red crystals with iced absolute ethyl alcohol, and drying the washed red crystals, thereby obtaining the (1,5-cyclooctadiene)-dichloro iridium dipolymer; and performing vacuum concentration treatment on filtrate so as to respectively recover noble metal iridium and a solvent. Compared with an existing synthesis method, the synthesis method disclosed by the invention has the advantages that the reaction time is greatly shortened, the synthesis method is simple in operation with one-step reaction, and the productivity is greatly improved; the one-step synthesis method can be used for solving the defects of overlong reaction time, strict reaction conditions, raw material waste and the like in an existing synthesis process, and has the advantages of environmental conservation, economical efficiency, simplicity and convenience in operation, relatively short reaction time and the like.

Description

technical field [0001] The invention relates to a preparation method of a noble metal catalyst using 1,5-cyclooctadiene as a ligand, in particular to a one-step direct synthesis method of (1,5-cyclooctadiene)-dichloroiridium dimer. Background technique [0002] Due to its unique d-electron configuration of platinum group elements, iridium atoms can form a special structure of organometallic complexes, thereby promoting many chemical reactions to proceed smoothly. catalyst. [0003] Chlorine-bridged dinuclear complex (1,5-cyclooctadiene)-dichloroiridium dimer ([Ir(COD)Cl] 2 ) is an important noble metal catalyst, due to its unique catalytic properties, [Ir(COD)Cl] 2 As a catalyst, it has the advantages of a wide range of applicable substrates, easy access to raw materials, high enantioselectivity, and multiple catalytic effects. Therefore, [Ir(COD)Cl] 2 As a homogeneous catalyst, it has attracted widespread attention from academia and industry. After research and testing,...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/0033
Inventor 高传柱余从涛张艳
Owner KUNMING UNIV OF SCI & TECH
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