Preparation method of 10 'H-spiro [fluorene-9, 9'-phenanthrene]-10 '-ketone

A technology of fluorenone and triethyl phosphite, which is applied in the field of organic synthesis, can solve the problems of not being able to meet industrialized large-scale production, environmental protection, low reaction efficiency, and uneconomical preparation process, and achieve less emissions, reduced emissions, The effect of simple operation of the reaction

Pending Publication Date: 2022-03-15
维思普新材料(苏州)有限公司
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a preparation method of 10'H-spiro[fluorene-9,9'-phenanthrene]-10'-one, the purpose of which is to solve the problem of 10'H-spiro[fluorene-9,9'-phenanthrene-9,9 The pr

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
  • Preparation method of 10 'H-spiro [fluorene-9, 9'-phenanthrene]-10 '-ketone
  • Preparation method of 10 'H-spiro [fluorene-9, 9'-phenanthrene]-10 '-ketone
  • Preparation method of 10 'H-spiro [fluorene-9, 9'-phenanthrene]-10 '-ketone

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0038] Example 1

[0039] Preparation of 10'H-spiro[fluorene-9,9'-phenanthrene]-10'-one

[0040] 1) Add 200 g of triethyl phosphite to a 1L four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, and start stirring. Under low-speed stirring, 100 g of fluorenone was added into the reaction flask. After the system was evenly stirred, the temperature was raised to reflux, and the reaction was kept for 24 hours. During the reaction process, the material gradually dissolves, and the color of the solution gradually deepens;

[0041] 2) After the reaction is completed, the heating is stopped, and the reaction is cooled to 100 ℃ by itself. When the temperature dropped to room temperature, a large amount of white crystals separated out in the reaction bottle and were collected by suction filtration;

[0042] 3) Transfer the solid to another 1L four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, add anhydrous ethanol twice the weig...

Example Embodiment

[0044] Example 2

[0045] Preparation of 10'H-spiro[fluorene-9,9'-phenanthrene]-10'-one

[0046] 1) Add 250 g of triethyl phosphite to a 1L four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, and start stirring. Under low-speed stirring, 100 g of fluorenone was added into the reaction flask. After the system was evenly stirred, the temperature was raised to reflux, and the reaction was kept for 24 hours. During the reaction process, the material gradually dissolves, and the color of the solution gradually deepens;

[0047] 2) After the reaction is completed, the heating is stopped, and the reaction is cooled to 100 ℃ by itself. When the temperature dropped to room temperature, a large amount of white crystals separated out in the reaction bottle and were collected by suction filtration;

[0048] 3) Transfer the solid to another 1L four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, add anhydrous ethanol twice the we...

Example Embodiment

[0050] Example 3

[0051] Preparation of 10'H-spiro[fluorene-9,9'-phenanthrene]-10'-one

[0052] 1) Add 300 g of triethyl phosphite to a 1L four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, and start stirring. Under low-speed stirring, 100 g of fluorenone was added into the reaction flask. After the system was evenly stirred, the temperature was raised to reflux, and the reaction was kept for 24 hours. During the reaction process, the material gradually dissolves, and the color of the solution gradually deepens;

[0053] 2) After the reaction is completed, the heating is stopped, and the reaction is cooled to 100 ℃ by itself. When the temperature dropped to room temperature, a large amount of white crystals separated out in the reaction bottle and were collected by suction filtration;

[0054] 3) Transfer the solid to another 1L four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, add anhydrous ethanol twice the we...

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 provides a preparation method of 10 'H-spiro [fluorene-9, 9'-phenanthrene]-10 '-ketone, which comprises the following steps: 1) adding fluorenone into a triethyl phosphite solvent, and uniformly stirring for reaction; 2) after the reaction, cooling to room temperature, and performing suction filtration to obtain a solid substance; 3) adding the solid substance into absolute ethyl alcohol, refluxing and pulping, cooling, crystallizing, filtering, washing and drying to obtain 10 'H-spiro [fluorene-9, 9'-phenanthrene]-10 '-ketone; and 4) distilling to obtain residues, adding the filtrate in the step 3), refluxing, pulping, cooling, crystallizing, filtering, washing and drying to obtain the 10 'H-spiro [fluorene-9, 9'-phenanthrene]-10 '-ketone.The preparation method disclosed by the invention is simple in reaction operation, easy in product purification, small in waste discharge amount, small in environmental pollution and suitable for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of 10'H-spiro[fluorene-9,9'-phenanthrene]-10'-one. Background technique [0002] 10'H-spiro[fluorene-9,9'-phenanthrene]-10'-one is a kind of organic compound with special spatial structure, its molecule has both the classic 9,9'-spirobifluorene molecular skeleton and carbonyl Functional groups and unique molecular structure make 10′H-spiro[fluorene-9,9′-phenanthrene]-10′-one have many special properties. While retaining the spiro ring structure, the presence of the carbonyl endows the molecule with a certain ability to pull electrons, which can improve the electron transport performance of the molecule to a certain extent (Journal of Power Sources, 2020, 458, 228063; Organic Electronics, 2019, 65, 135-140 ; ChemSusChem, 2018, 11, 3225-3233.). The existence of the carbonyl group allows the transformation of the functional group of the molecule. 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
IPC IPC(8): C07C45/00C07C45/81C07C49/665
CPCC07C45/00C07C45/81C07C2603/94C07C49/665
Inventor 刘向阳张业欣袁晓冬陈华
Owner 维思普新材料(苏州)有限公司
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