A kind of diamine compound containing m-terphenyl structure and its synthesis method and application
A technology for m-terphenyl and amine compounds, which is applied to diamine compounds containing m-terphenyl structure and the fields of synthesis and application thereof, can solve the problems of difficult processing and molding, application limitation, insoluble and insoluble polyimide, etc. Interaction force, improved solubility, easy purification effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0036] Example 1: Synthesis of 5'-(4-(trifluoromethyl)phenyl)-[1,1':3',1"-terphenyl]-3,3"-diamine
[0037] (1) In a three-necked flask, add 11.25g (50mmol) of 4-bromobenzotrifluoride, 9.54g (55mmol) of p-aminophenyl borate hydrochloride, 75ml of 2mol / L potassium carbonate solution and 250ml of tetrahydrofuran, magnetically stir and pass Argon, after heating the oil bath to 75°C, add 0.02g tetrakistriphenylphosphine palladium, reflux for 12h and then let it stand, separate the liquid to remove the water layer, then mix with silica gel and spin dry to pass through the chromatographic column, collect the product point solution and spin dry to get white The solid was dried in vacuum at 60° C. for 12 h to obtain 11.3 g of a white intermediate product 4-Amino-4'-(trifluoromethyl)-1,1'-biphenyl with a yield of 95%. The intermediate structure is as follows:
[0038]
[0039] (2) In a three-necked flask, add 4-Amino-4'-(trifluoromethyl)-1,1'-biphenyl 7.12g (30mmol) and 30ml of DMF ...
Embodiment 2
[0049] Example 2: Synthesis of 5'-(4-fluorophenyl)-[1,1':3',1″-terphenyl]-3,3″-diamine
[0050] (1) In a three-necked flask, add 8.75g (50mmol) of 4-bromofluorobenzene, 9.54g (55mmol) of p-aminophenyl borate hydrochloride, 75ml of 2mol / L potassium carbonate solution, a few drops of phase transfer catalyst and 250ml of tetrahydrofuran , magnetic stirring and argon gas, after heating the oil bath to 75°C, add 0.02g tetrakistriphenylphosphine palladium, reflux for 12h, let stand for liquid separation to remove the water layer, then mix with silica gel and spin dry, pass through the chromatography column, and collect the product point The solution was spin-dried to obtain a white solid, which was dried in vacuum at 60°C for 12 hours to obtain 8.61 g of a white intermediate product 4'-fluoro-[1,1'-biphenyl]-4-amine with a yield of 92%. The intermediate structure is as follows:
[0051]
[0052] (2) In a three-necked flask, add 5.62g (30mmol) of 4'-fluoro-[1,1'-biphenyl]-4-amine...
Embodiment 3
[0062] Example 3: Synthesis of 5'-(3,5-bis(trifluoromethyl)phenyl)-[1,1':3',1″-terphenyl]-3,3″-diamine
[0063] (1) In a three-necked flask, add 1-bromo-3,5-bis(trifluoromethyl)benzene14.65g (50mmol), p-aminophenyl borate hydrochloride 9.54g (55mmol), 2mol / L potassium carbonate solution 75ml and 250ml tetrahydrofuran, magnetically stirred and argon, heated to 75°C in an oil bath, added 0.02g tetrakistriphenylphosphine palladium, refluxed for 12 hours, left to separate liquids to remove the water layer, mixed with silica gel, spin-dried, and passed through the chromatography column. The collected product point solution was spin-dried to obtain a white solid, which was dried in vacuum at 60°C for 12 hours to obtain 14.50 g of the white intermediate product 3',5'-bis(trifluoro-methyl)-[1,1'-biphenyl]-4-amine. The rate is 94%. The intermediate structure is as follows:
[0064]
[0065] (2) In a three-necked flask, add 3',5'-bis(trifluoromethyl)-[1,1'-biphenyl]-4-amine9.16g (3...
PUM
| Property | Measurement | Unit |
|---|---|---|
| melting point | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More 