Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Co-crystal formed by 2,2',3,3'-tetrahydroxy dinaphthalene and 4,4'-dipyridyl and preparation method

A technology of hydroxybinaphthalene and bipyridine, which is applied in the field of co-crystals between polyphenolic compounds and pyridine-containing compounds, can solve the problem that the formation mechanism of co-crystals is not fully grasped, etc.

Inactive Publication Date: 2017-08-18
LUOYANG NORMAL UNIV
View PDF2 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first challenge encountered is that the formation mechanism of eutectic formation is not fully grasped, mainly because not any two components can form eutectics, so there must be which components can form crystals and how many components there are Ability to co-assemble crystallization, etc.

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
  • Co-crystal formed by 2,2',3,3'-tetrahydroxy dinaphthalene and 4,4'-dipyridyl and preparation method
  • Co-crystal formed by 2,2',3,3'-tetrahydroxy dinaphthalene and 4,4'-dipyridyl and preparation method
  • Co-crystal formed by 2,2',3,3'-tetrahydroxy dinaphthalene and 4,4'-dipyridyl and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 1.0 mmol 2,2',3,3'-tetrahydroxy-1,1'-binaphthyl (318 mg), 1.0 mmol 4,4'-bipyridine (156 mg) in a 50 mL round bottom flask, The molar ratio of the two was 1:1, and then 30 mL of acetonitrile was added, and the solid accounted for 2.0% of the total mass of the system. Put a magnet, install a reflux condenser, heat and reflux for 1 hour under stirring, filter while it is hot, and let the filtrate volatilize naturally at room temperature. After a few days, a large number of colorless crystals are precipitated from the filtrate. 30 h 22 N 2 o 4 The eutectic had a weighed mass of 455 mg and a yield of 96%.

[0028] The characterization process of the eutectic formed by 2,2’,3,3’-tetrahydroxy-1,1’-binaphthalene and 4,4’-bipyridine is as follows:

[0029] (1) Determination of the eutectic single crystal structure of 2,2',3,3'-tetrahydroxy-1,1'-binaphthyl and 4,4'-bipyridine

[0030] Select crystals of appropriate size and stick them on a glass filament, and place them ...

Embodiment 2

[0035] Put 2.0 mmol 2,2',3,3'-tetrahydroxy-1,1'-binaphthyl (636 mg), 1.0 mmol 4,4'-bipyridyl (156 mg) in a 50 mL round bottom flask, The molar ratio of the two was 2:1, and then 30 mL of acetonitrile was added, and the solid accounted for 3.3% of the total mass of the system. Put a magnet, install a reflux condenser, heat and reflux for 1 hour under stirring, filter while it is hot, and let the filtrate volatilize naturally at room temperature. After a few days, a large number of colorless crystals are precipitated from the filtrate.30 h 22 N 2 o 4 The eutectic had a weighed mass of 446 mg and a yield of 94%.

Embodiment 3

[0037] Put 1.0 mmol 2,2',3,3'-tetrahydroxy-1,1'-binaphthyl (318 mg), 2.0 mmol 4,4'-bipyridyl (312 mg) in a 50 mL round bottom flask, The molar ratio of the two was 1:2, and then 30 mL of acetonitrile was added, and the solid accounted for 2.6% of the total mass of the system. Put a magnet, install a reflux condenser, heat and reflux for 1 hour under stirring, filter while it is hot, and let the filtrate volatilize naturally at room temperature. After a few days, a large number of colorless crystals are precipitated from the filtrate. 30 h 22 N 2 o 4 The eutectic had a weighed mass of 431 mg and a yield of 91%.

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 co-crystal formed by 2,2',3,3'-tetrahydroxy dinaphthalene and 4,4'-dipyridyl and a preparation method. The preparation method comprises the following steps: forming a co-crystal basic structure unit with one 2,2',3,3'-tetrahydroxy-1,1'-dinaphthalene molecule and one 4,4'-dipyridyl molecule through the action of O-H...N hydrogen bonds; forming a one-dimensional helical chain with the 2,2',3,3'-tetrahydroxy-1,1'-dinaphthalene molecule in the co-crystal through an O-H...O hydrogen bond between every two adjacent molecules; connecting the 4, 4'-dipyridyl molecule on the one-dimensional helical chain an O-H...N hydrogen bond to form a two-dimensional layered structure, wherein the overall structure of the co-crystal is the helical chain clathrate 4,4'-dipyridyl molecule formed by the 2,2',3,3'-tetrahydroxy-1,1'-dinaphthalene molecule. In the preparation method, the co-crystal is prepared by adopting a solution cooling crystallization method by taking acetonitrile and trichloromethane as solvents. The invention provides the preparation method for forming the co-crystal with polyphenol and a pyridine substance, so that a theoretical guiding significance is provided for preparation of the type of pharmaceutical co-crystals.

Description

technical field [0001] The invention belongs to the technical field of co-crystals of polyphenolic compounds and pyridine-containing compounds, and specifically relates to a co-crystal of 2,2',3,3'-tetrahydroxybinaphthalene and 4,4'-bipyridine and Preparation. Background technique [0002] The first co-crystal was the hydroquinone co-crystal prepared by WÖhler in 1844. In 1967, Schmidt and Snipes first used the term "co-crystal" to describe the compound molecule of pyrimidine and purine. Since then, the concept of eutectic has been constantly updating its meaning. Until 2003, a more generally accepted concept is eutectic as a homogeneous crystalline material, which contains two or more stoichiometric neutral components. [0003] The concepts of supramolecular chemistry and crystal engineering believe that cocrystal is a kind of supramolecular self-assembly system, which is the most stable result of the interaction among thermodynamics, kinetics and molecular recognition to ...

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
IPC IPC(8): C07D213/22C07D213/127C07C37/00C07C39/14
CPCC07B2200/13C07C37/00C07C39/14C07D213/127C07D213/22
Inventor 吉保明邓冬生
Owner LUOYANG NORMAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com