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A kind of catalyst for the reaction of 4-iodonitrobenzene and phenylacetylene

A catalyst, dimethylacetamide technology, applied in the direction of physical/chemical process catalysts, catalytic reactions, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of poor stability of solid catalysts, inability to recycle multiple times, Problems such as the decline in catalytic efficiency of solid catalysts

Active Publication Date: 2021-11-16
SOUTHERN MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are also related solid catalysts in the prior art, but the catalytic efficiency is low, so that the yield of the target product is too low, and the related solid catalysts have poor stability and cannot be recycled multiple times, or as the number of times of recycling increases, the solid Catalytic efficiency drops rapidly

Method used

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  • A kind of catalyst for the reaction of 4-iodonitrobenzene and phenylacetylene
  • A kind of catalyst for the reaction of 4-iodonitrobenzene and phenylacetylene
  • A kind of catalyst for the reaction of 4-iodonitrobenzene and phenylacetylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1: the preparation of catalyst

[0053] A solid catalyst comprises a carrier and an active component, the carrier is zirconium hydrogen phosphate, and the active component is a ferrocene group.

[0054] The zirconium hydrogen phosphate exists in the catalyst in the form of single-layer zirconium hydrogen phosphate nanosheets.

[0055] The ferrocene group is introduced into the catalyst in the form of 1-hydroxyethylferrocene.

[0056] In terms of molar ratio, the molar ratio of zirconium hydrogen phosphate to ferrocene group is 85:15.

[0057] The zirconium hydrogen phosphate is connected to the ferrocene group through isocyanate propyltriethoxysilane.

[0058] A preparation method of catalyst, comprising the following steps:

[0059] (1) Add 1-hydroxyethylferrocene and propyltriethoxysilane isocyanate to DMAC (dimethylacetamide), react for 2 hours, and stir constantly during the reaction to obtain product A, set aside , the reaction equation is as follows...

Embodiment 2

[0073] Embodiment 2: the preparation of catalyst

[0074] A solid catalyst comprises a carrier and an active component, the carrier is zirconium hydrogen phosphate, and the active component is a ferrocene group.

[0075] The zirconium hydrogen phosphate exists in the catalyst in the form of layered zirconium hydrogen phosphate nanosheets.

[0076] The ferrocene group is introduced into the catalyst in the form of 1-hydroxyethylferrocene.

[0077] The catalyst, in terms of molar ratio, has a molar ratio of zirconium hydrogen phosphate to ferrocene group of 80:15.

[0078] The zirconium hydrogen phosphate is connected to the ferrocene group through isocyanate propyltriethoxysilane.

[0079] A preparation method of catalyst, comprising the following steps:

[0080] (1) Add 1-hydroxyethylferrocene and propyltriethoxysilane isocyanate to DMAC (dimethylacetamide), react for 1.5 hours, stir continuously during the reaction, and obtain product A, set aside , the reaction equation ...

Embodiment 3

[0093] Embodiment 3: Preparation of 1-iodo-4-(2-phenylethynyl)benzene

[0094] The catalyst prepared in Example 1 is used to catalyze the reaction of 4-iodonitrobenzene and phenylacetylene to generate 1-iodo-4-(2-phenylethynyl)benzene, and the equation of the reaction is as follows:

[0095]

[0096] The reaction of 4-iodonitrobenzene and phenylacetylene to generate 1-iodo-4-(2-phenylethynyl)benzene is carried out in the solvent DMAC.

[0097] The catalyst, 4-iodonitrobenzene and phenylacetylene are used in a molar ratio of 0.1:1:1.

[0098] The molar ratio of the catalyst to DMAC is 0.1:5.

[0099] The reaction temperature is 70° C., the reaction pressure is normal pressure, and the reaction time is 8 hours.

[0100] In the reaction, the reaction device is a batch reactor.

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Abstract

The invention belongs to the field of organic synthesis and discloses a solid catalyst comprising zirconium hydrogen phosphate and a ferrocene group, the zirconium hydrogen phosphate is a carrier, and the ferrocene group is an active component; in molar ratio, The molar ratio of the zirconium hydrogen phosphate to the ferrocene group is 80-90:10-20; the zirconium hydrogen phosphate and the nitrite group are connected through a silyl group. Compared with the prior art, the catalyst of the present invention is a solid catalyst, which makes the separation and purification of the product very easy; the reaction of catalyzed 4-iodonitrobenzene and phenylacetylene with the catalyst of the present invention generates 1-iodine-4-(2 -phenylethynyl)benzene, the productive rate of 1-iodo-4-(2-phenylethynyl)benzene can be as high as 98.5%, and the conversion rate of 4-iodonitrobenzene is as high as 100%; the catalyst can be recycled many times .

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a catalyst for the reaction of 4-iodonitrobenzene and phenylacetylene. Background technique [0002] The reaction of 4-iodonitrobenzene and phenylacetylene is a basic reaction in chemistry, and the 1-iodo-4-(2-phenylethynyl)benzene produced by the reaction has important applications (1-iodo-4-(2-benzene Ethynyl)benzene is an important active intermediate in the process of drug synthesis, and is also an important intermediate in the synthesis of some functional materials). In the prior art, the catalysts that catalyze the reaction between 4-iodonitrobenzene and phenylacetylene generally have low catalytic efficiency, and the catalysts are gradually deactivated as the reaction proceeds, so the catalysts are difficult to reuse. Most of the catalysts in the prior art that catalyze the reaction between 4-iodonitrobenzene and phenylacetylene are liquid catalysts. After the reaction is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/38C07C17/263C07C25/24
CPCB01J31/2295B01J31/38B01J2231/4205B01J2531/842C07C17/263C07C25/24Y02P20/584
Inventor 张蒙张翠兰
Owner SOUTHERN MEDICAL UNIVERSITY