1,1-dipyrazolemethane binuclear manganese polymer and its in-situ decarboxylation synthesis method and application

A dipyrazolemethane and synthesis method technology, which is applied in the field of in-situ decarboxylation synthesis of 1,1-dipyrazolemethane binuclear manganese polymers, can solve the problems of low conversion rate and slow reaction speed, and achieve low cost and good conditions Gentle and stable effect

Active Publication Date: 2018-11-06
SOUTHEAST UNIV
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the reported heterogeneous catalysts for silylation, such as binuclear dimeric Salen titanium complex catalysts, copper metal complex framework catalysts, etc., have the disadvantages of low conversion rate and slow reaction rate.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 1,1-dipyrazolemethane binuclear manganese polymer and its in-situ decarboxylation synthesis method and application
  • 1,1-dipyrazolemethane binuclear manganese polymer and its in-situ decarboxylation synthesis method and application
  • 1,1-dipyrazolemethane binuclear manganese polymer and its in-situ decarboxylation synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) 0.197 grams of analytically pure MnCl 2 4H 2 O and 0.192 grams of analytically pure 1,1-dipyrazole acetic acid were dissolved in 10 milliliters of anhydrous acetonitrile;

[0026] (2) The solution in step (1) was stirred at room temperature for 5 minutes until all reactants were dissolved and clarified;

[0027] (3) Transfer the solution prepared in step (2) to a polytetrafluoroethylene reactor and react at 110°C for 100 hours, cool down to room temperature, open the kettle, filter, and wash with anhydrous acetonitrile to obtain single crystal grade 1,1 -Dipyrazolemethane binuclear manganese polymer, yield 78-85%.

[0028] And confirm its structural formula with X-ray single crystal diffraction, infrared spectrum, mass spectrum, nuclear magnetic resonance proton spectrum / carbon spectrum as:

[0029]

[0030] The basic data of the resulting 1,1-dipyrazolemethane binuclear manganese polymers were analyzed:

[0031] X-ray single crystal diffraction characterizat...

Embodiment 2

[0033] (1) 0.256 gram of analytically pure MnCl 2 4H 2 O and 0.245 grams of analytically pure 1,1-dipyrazole acetic acid were dissolved in 12 milliliters of anhydrous acetonitrile;

[0034] (2) The solution in step (1) was stirred at room temperature for 5 minutes until all reactants were dissolved and clarified;

[0035] (3) Transfer the solution prepared in step (2) to a polytetrafluoroethylene reactor and react at 120°C for 120 hours, cool down to room temperature, open the kettle, filter, and wash with anhydrous acetonitrile to obtain single crystal grade 1,1 -Dipyrazolemethane binuclear manganese polymer, yield 78-85%.

Embodiment 3

[0037] (1) 0.380 gram of analytically pure MnCl 2 4H 2 O and 0.360 grams of analytically pure 1,1-dipyrazole acetic acid are dissolved in 15 milliliters of anhydrous acetonitrile;

[0038] (2) Stir the solution in step (1) at room temperature for 10 minutes until all reactants are dissolved and clarified;

[0039] (3) Transfer the solution prepared in step (2) to a polytetrafluoroethylene reactor and react at 140°C for 150 hours, cool down to room temperature, open the kettle, filter, and wash with anhydrous acetonitrile to obtain single crystal grade 1,1 -Dipyrazolemethane binuclear manganese polymer, yield 78-85%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a 1,1-dipyrazole methane duel-core manganese polymer and further provides an in-situ decarboxylation synthetic method and application thereof. The polymer has the advantages that the process is simple, the cost is low, the chemical components are easy to control, the repeatability is good, the yield is high, the catalytic effect is excellent, and the like.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and catalytic application, and in particular relates to an in-situ decarboxylation synthesis method and application of a 1,1-dipyrazolemethane binuclear manganese polymer. Background technique [0002] Asymmetric silylation reaction is a kind of asymmetric catalytic synthesis reaction developed in recent years, which is mainly used to synthesize chiral cyanohydrins. Chiral cyanohydrins are a class of organic synthesis intermediates with a wide range of uses. Its two functional groups undergo multi-step transformations to synthesize a series of optically pure chiral products, namely α-hydroxy acids, α-hydroxy aldehydes, α-hydroxy ketones, β-hydroxylamines, α-amino acids, etc.; cyanohydrins are also the starting materials for the synthesis of many drugs, such as cardiovascular dilating drugs; cyanohydrins are also important constituent fragments of some natural products and pesticides, for example,...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C07F13/00B01J31/22C07F7/18
CPCB01J31/1815B01J2231/34B01J2531/0205B01J2531/0216B01J2531/0238B01J2531/72C07F7/1804C07F13/005
Inventor 赵红江道勇冯超薛兴颖
Owner SOUTHEAST UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap