PL433408A1 - 2,3-diphenyl-N,N'-bis(2,6-diisopropylphenyl)benzo[ghi]perylenediimide and method of its preparation - Google Patents

2,3-diphenyl-N,N'-bis(2,6-diisopropylphenyl)benzo[ghi]perylenediimide and method of its preparation

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Publication number
PL433408A1
PL433408A1 PL433408A PL43340820A PL433408A1 PL 433408 A1 PL433408 A1 PL 433408A1 PL 433408 A PL433408 A PL 433408A PL 43340820 A PL43340820 A PL 43340820A PL 433408 A1 PL433408 A1 PL 433408A1
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PL
Poland
Prior art keywords
diisopropylphenyl
bis
saturated
benzo
diphenyl
Prior art date
Application number
PL433408A
Other languages
Polish (pl)
Other versions
PL241965B1 (en
Inventor
Stanisław Krompiec
Grażyna Szafraniec-Gorol
Marek Matussek
Witold Ignasiak
Michał Filapek
Original Assignee
Uniwersytet Śląski W Katowicach
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Uniwersytet Śląski W Katowicach filed Critical Uniwersytet Śląski W Katowicach
Priority to PL433408A priority Critical patent/PL241965B1/en
Publication of PL433408A1 publication Critical patent/PL433408A1/en
Publication of PL241965B1 publication Critical patent/PL241965B1/en

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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells

Abstract

Przedmiotem wynalazku jest 2,3-difenylo-N,N'-bis(2,6-diizopropylofenylo)benzo[ghi]perylenodiimid przedstawiony wzorem 1 oraz sposób jego otrzymywania polegający na tym, że do reaktora odpornego na nadciśnienie wprowadza się N,N'-bis(2,6-diizopropylofenylo)perylenodiimid oraz 1,2-difenyloacetylen w proporcjach molowych od 1:2 do 1:50, reaktor zamyka się i wytwarza w nim próżnię, po czym prowadzi się reakcję w temperaturze od 260 do 310°C, przez czas nie krótszy niż 24 godziny, a po zakończeniu reakcji cykloaddycji 2,3-difenylo-N,N'-bis(2,6-diizopropylofenylo)benzo[ghi]perylenodiimid wydziela się w dwojaki sposób, to jest albo: a) nadmiarowy 1,2-difenyloacetylen usuwa się za pomocą próżniowej sublimacji w znany sposób, a z pozostałości po sublimacji izoluje się produkt chromatograficznie, na kolumnie z żelem krzemionkowym, przy czym najpierw eluuje się pozostałości nieprzereagowanego difenyloacetylenu i niektóre zanieczyszczenia za pomocą niskowrzącego, nasyconego, ciekłego węglowodoru lub mieszaniny ciekłych węglowodorów nasyconych, a finalnie produkt, to jest 2,3-difenylo-N,N'-bis(2,6-diizopropylofenylo)benzo[ghi]perylenodiimid eluuje się za pomocą niskowrzącego, nasyconego, ciekłego węglowodoru zmieszanego z dichlorometanem lub chloroformem lub mieszaniny ciekłych węglowodorów nasyconych, zmieszanych z dichlorometanem lub chloroformem, w proporcjach objętościowych rozpuszczalnik węglowodorowy/rozpuszczalnik chlorowany od 1:1 do 1:100, albo: b) nadmiarowy 1,2-difenyloacetylen usuwa się eluując go chromatograficznie, na kolumnie z żelem krzemionkowym, ciekłym, nasyconym węglowodorem lub mieszaniną nasyconych, ciekłych węglowodorów, a finalnie produkt, to jest 2,3-difenylo-N,N'-bis(2,6-diizopropylofenylo)benzo[ghi]perylenodiimid eluuje się za pomocą niskowrzącego, nasyconego, ciekłego węglowodoru zmieszanego z dichlorometanem lub chloroformem lub mieszaniny ciekłych węglowodorów nasyconych, zmieszanych z dichlorometanem lub chloroformem, proporcjach objętościowych rozpuszczalnik węglowodorowy/rozpuszczalnik chlorowany od 1:1 do 1:100. Produkt reakcji może być luminoforem, prekursorem nanografenów lub nanomateriałów dla organicznej elektroniki, składnikiem warstw aktywnych, na przykład w OLED-ach lub substratem dla dalszych cykloaddycji lub cyklo-dehydrokondensacji.The subject of the invention is 2,3-diphenyl-N, N'-bis (2,6-diisopropylphenyl) benzo [gh] perylene diimide represented by the formula 1, and a method for its preparation consisting in introducing N, N 'into an overpressure-resistant reactor -bis (2,6-diisopropylphenyl) perylene diimide and 1,2-diphenylacetylene in molar proportions from 1: 2 to 1:50, the reactor is closed and a vacuum is created in it, and the reaction is carried out at a temperature of 260 to 310 ° C , for a time not shorter than 24 hours, and after the cycloaddition reaction is completed, 2,3-diphenyl-N, N'-bis (2,6-diisopropylphenyl) benzo [ghi] perylene diimide is isolated in two ways, that is either: a) the excess 1,2-diphenylacetylene is removed by vacuum sublimation in a known manner, and the product is isolated from the sublimation residue by chromatography on a silica gel column, first eluting unreacted diphenylacetylene residues and some impurities with a low-boiling, saturated liquid hydrocarbon NS or mixtures of saturated liquid hydrocarbons and finally the product, i.e. 2,3-diphenyl-N, N'-bis (2,6-diisopropylphenyl) benzo [gh] perylene diimide, is eluted with a low-boiling saturated liquid hydrocarbon mixed with dichloromethane or with chloroform or a mixture of saturated liquid hydrocarbons mixed with dichloromethane or chloroform, in the proportions by volume hydrocarbon solvent / chlorinated solvent from 1: 1 to 1: 100, or: b) the excess 1,2-diphenylacetylene is removed by chromatography elution on a gel column silica, liquid, saturated hydrocarbon or a mixture of saturated liquid hydrocarbons, and the final product, i.e. 2,3-diphenyl-N, N'-bis (2,6-diisopropylphenyl) benzo [ghi] perylene diimide, is eluted with low boiling, saturated , liquid hydrocarbon mixed with dichloromethane or chloroform, or a mixture of liquid saturated hydrocarbons mixed with dichloromethane or chloroform, the proportions by volume of dilution hydrocarbon solvent / chlorinated solvent from 1: 1 to 1: 100. The reaction product may be a phosphor, a nanografen or nanomaterials precursor for organic electronics, a component of active layers, for example in OLEDs, or a substrate for further cycloaddition or cyclo-dehydrocondensation.

PL433408A 2020-03-31 2020-03-31 2,3-diphenyl-N,N'-bis(2,6-diisopropylphenyl)benzo[ghi]perylenediimide and method of its preparation PL241965B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL433408A PL241965B1 (en) 2020-03-31 2020-03-31 2,3-diphenyl-N,N'-bis(2,6-diisopropylphenyl)benzo[ghi]perylenediimide and method of its preparation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PL433408A PL241965B1 (en) 2020-03-31 2020-03-31 2,3-diphenyl-N,N'-bis(2,6-diisopropylphenyl)benzo[ghi]perylenediimide and method of its preparation

Publications (2)

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PL433408A1 true PL433408A1 (en) 2021-10-04
PL241965B1 PL241965B1 (en) 2023-01-02

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