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A kind of catalyst composition and its application

A composition and compound technology, applied in physical/chemical process catalysts, chemical/physical process, organic compound/hydride/coordination complex catalysts, etc., can solve unseen problems

Inactive Publication Date: 2017-06-30
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, there is no report on the preparation of 2,4-quinazolinedione compounds by the reaction of 2-aminobenzonitrile compounds and carbon dioxide catalyzed by amide group divalent rare earth metal amides, and there is no report on amide group divalent rare earth metal amides A report on the preparation of 2,4-quinazolinediones by the reaction of 2-aminobenzonitriles and carbon dioxide catalyzed by DBU

Method used

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  • A kind of catalyst composition and its application
  • A kind of catalyst composition and its application
  • A kind of catalyst composition and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1 {L 1 Eu[N(SiMe 3 ) 2 ]·THF} 2 preparation of

[0065] In an anhydrous, oxygen-free, argon-protected reaction flask, add Eu[N(SiMe 3 ) 2 ] 2 , dissolved in tetrahydrofuran; in another anhydrous, oxygen-free, argon-protected reaction flask, weigh and Eu[N(SiMe 3 ) 2 ] 2 Equimolar ratio of ligand L 1 H, add tetrahydrofuran, slowly add the ligand solution to Eu[N(SiMe 3 ) 2 ] 2 In the clear solution of ether solvent, react for 4h, and finally obtain the clear solution.

[0066] After the reaction, drain the solvent, wash with n-hexane, then add tetrahydrofuran until completely dissolved, centrifuge, take the supernatant into a crystallization bottle, drain the solvent, dissolve with an appropriate amount of tetrahydrofuran-n-hexane, and stand at room temperature until crystals are precipitated , that is, amido divalent rare earth amides {L 1 Eu[N(SiMe 3 ) 2 ]·THF} 2 , the yield was 75%.

[0067] {L 1 Eu[N(SiMe 3 ) 2 ]·THF} 2 See Table 1 for...

Embodiment 2

[0074] Example 2 {L 2 Yb[N(SiMe 3 ) 2 ]·THF} 2 preparation of

[0075] Add Yb[N(SiMe 3 ) 2 ] 2 , dissolved in tetrahydrofuran; weighed and Yb[N(SiMe 3 ) 2 ] 2 Equimolar ratio of ligand L 2 H, add tetrahydrofuran, slowly add the ligand solution to Yb[N(SiMe 3 ) 2 ] 2 In the clear solution of ether solvent, react for 4h, and finally obtain the clear solution.

[0076] After the reaction, drain the solvent, wash with n-hexane, then add tetrahydrofuran until completely dissolved, centrifuge, take the supernatant into a crystallization bottle, drain the solvent, dissolve with an appropriate amount of tetrahydrofuran-n-hexane, and stand at room temperature until crystals are precipitated , that is, amido divalent rare earth amides {L 2 Yb[N(SiMe 3 ) 2 ]·THF} 2 , the yield was 82%.

Embodiment 3

[0077] Example 3 {L 2 Eu[N(SiMe 3 ) 2 ]·THF} 2 preparation of

[0078] In an anhydrous, oxygen-free, argon-protected reaction flask, add Eu[N(SiMe 3 ) 2 ] 2 , dissolved in tetrahydrofuran; in another anhydrous, oxygen-free, argon-protected reaction flask, weigh the Eu[N(SiMe 3 ) 2 ] 2 Equimolar ratio of ligand L 2 H, add tetrahydrofuran, slowly add the ligand solution to Eu[N(SiMe 3 ) 2 ] 2 In the clear liquid of ether solvent, the clear liquid was finally obtained after reacting for 4 hours.

[0079] After the reaction, drain the solvent, wash with n-hexane, then add tetrahydrofuran until completely dissolved, centrifuge, take the supernatant into a crystallization bottle, drain the solvent, dissolve with an appropriate amount of tetrahydrofuran-n-hexane, and stand at room temperature until crystals are precipitated , that is, amido divalent rare earth amides {L 2 Eu[N(SiMe 3 ) 2 ]·THF} 2 , the yield was 78%.

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Abstract

The invention belongs to the field of organic chemistry, and concretely relates to a composition for catalyzing 2-aminobenzonitrile compound and carbon dioxide to react to prepare 2, 4-quinazoline diketone compound. According to catalysis of 2-aminobenzonitrile compound and carbon dioxide and a preparation of benzoyleneurea by reaction with carbon dioxide, the composition of acylamino divalent rare earth metal amide combined with DBU used as a catalyst has a catalysis yield which is higher than the catalysis yield of acylamino divalent rare earth metal amide which is used individually or DBU which is used individually, and the composition of acylamino divalent rare earth metal amide combined with DBU has a cooperative catalysis effect.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and specifically relates to a composition for catalyzing the reaction of 2-aminobenzonitrile compounds and carbon dioxide to prepare 2,4-quinazolinedione compounds and an application thereof. Background technique [0002] 2,4-Quinazolinedione compounds are an important class of dominant structural skeletons with a wide range of biological activities, for example, they can be used as antibiotics, serum receptor antagonists, glutamate receptor antagonists, aldose reduction Enzyme inhibitors, calcium ion channel antagonists, acetylcholine receptor antagonists, etc. [0003] At present, there are many methods for preparing 2,4-quinazolinedione compounds. Among them, an important one is prepared by using carbon dioxide and 2-aminobenzonitrile compounds as raw materials under the action of a catalyst. This reaction has attracted much attention due to its atom economy. [0004] In 2002, Takumi Mizuno'...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07D239/96
Inventor 赵蓓王千宇陆澄容
Owner SUZHOU UNIV
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