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Basic heterogeneous catalyst for nitroformylation reaction and preparation and application

A heterogeneous catalyst, nitrogen formyl technology, applied in the preparation of organic compounds, catalysts for physical/chemical processes, preparation of carboxylic acid amides, etc., can solve the problems of harsh reaction conditions, low reaction activity, and difficulty in separating catalysts from reaction materials. , to achieve the effect of simple preparation method, high stability and excellent catalytic reaction performance

Active Publication Date: 2022-05-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The homogeneous catalytic system has higher catalytic activity and selectivity of the target product under milder reaction conditions, but it is difficult to separate the catalyst from the reaction material
Compared with homogeneous catalysis, the biggest advantage of heterogeneous catalysis is that the catalyst and the reaction materials are easy to separate. The main problems are harsh reaction conditions and relatively low reactivity.

Method used

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  • Basic heterogeneous catalyst for nitroformylation reaction and preparation and application
  • Basic heterogeneous catalyst for nitroformylation reaction and preparation and application
  • Basic heterogeneous catalyst for nitroformylation reaction and preparation and application

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Under 298K and argon protection atmosphere, 3.0 grams of tris (4-vinylphenyl) phosphine and 0.95 grams of sodium styrene sulfonate were dissolved in 50.0 ml of tetrahydrofuran solvent, and 0.075 grams of free radical initiator was added to the above solution. Azodiisobutyronitrile, stirred for 3 hours. The stirred solution was transferred to a hydrothermal autoclave, and polymerized by solvothermal method at 373K and an inert gas atmosphere for 24 hours. Cool to room temperature after the above-mentioned polymerization, and vacuum remove the solvent at 333K to obtain a porous organic copolymer containing triphenylphosphine and sodium sulfonate.

[0028] Under 298K and an inert gas protection atmosphere, weigh 0.0156 g of p-cymene dichloride ruthenium (II) dimer and dissolve it in 40 ml of tetrahydrofuran solvent, add 1.0 g of the above-mentioned preparation containing triphenylphosphine and sodium sulfonate Porous organic copolymer, stirred for 24 hours. Subsequently,...

Embodiment 2

[0030] In Example 2, in addition to weighing 0.078 gram of p-cymene dichloride ruthenium (II) dimer to replace 0.0156 gram of p-cymene dichloride ruthenium (II) dimer, the remaining catalyst preparation process and implementation Example 1 is the same.

Embodiment 3

[0032] In Example 3, except that 0.03 g of palladium acetate was weighed instead of 0.0156 g of p-cymene dichloride ruthenium (II) dimer, the rest of the catalyst preparation process was the same as in Example 1.

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Abstract

The present invention relates to a kind of heterogeneous catalyst with basicity and its preparation method and application, more particularly, relate to a kind of heterogeneous catalyst with basicity used in nitrogen formylation reaction, which is composed of metal component and organic ligand The composition of the copolymer, the organic ligand copolymer is a copolymer with a large specific surface area and a hierarchical pore structure produced by solvothermal copolymerization of a vinyl-functionalized phosphine ligand and a vinyl-functionalized organic base monomer . On the one hand, the catalyst of the present invention introduces an organic base into the copolymer carrier to make the solid heterogeneous catalyst alkaline, which promotes the positive movement of the nitrogen formylation reaction and improves the reactivity; on the other hand, the metal component and the P atom of the copolymer carrier Due to coordination, it is highly dispersed and stably exists on the carrier. Therefore, the basic heterogeneous catalyst of the present invention has excellent nitrogen formylation reaction performance and stability; and the catalyst is easy to separate from reactants and products, and has broad industrial application prospects.

Description

technical field [0001] The invention relates to a heterogeneous catalyst with basicity for nitrogen formylation reaction and its preparation method and application, belonging to the technical field of heterogeneous catalysis. Background technique [0002] The formylation reaction of amines is one of the important reactions in organic synthesis and medicinal chemistry. Formamide is an important intermediate in organic synthesis and is widely used in the synthesis of various drugs. Formamide can be used as raw material for organic synthesis, paper treatment agent, softener in the fiber industry, and as an analytical reagent for determining amino acid content in rice; at the same time, formamide is also an excellent organic solvent, which can be used to separate chlorosilanes and purify oil etc.; in addition, formamide has active reactivity and can undergo various reactions. In addition to the three hydrogens participating in the reaction, it can also undergo dehydration, deCO...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/24B01J35/10C07B43/06C07C231/10C07C233/03C07D295/185
CPCB01J35/1023B01J35/10B01J31/1691B01J31/2409C07B43/06C07C231/10C07D295/185B01J2531/821B01J2531/824B01J2531/847B01J2540/32C07C233/03
Inventor 丁云杰王国庆严丽姜淼程显波
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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