1, 6-disubstituted perylene diimide compound as well as synthesis method and application thereof
A technology of perylene diimide and synthesis method, which is applied in the field of 1,6-disubstituted perylene diimide compound and its synthesis, can solve problems such as difficulties in the synthesis of a large number of perylene diimide compounds, and achieve good industrial application Prospects, high photoelectric conversion efficiency, and easy-to-obtain raw materials
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[0038] The second aspect of the present invention provides a kind of synthetic method of 1,6-disubstituted perylene diimide compound, comprising the following steps:
[0039] S1. React compound 1 with anhydrous methanol under the action of the first base and the first organic solvent to obtain compound 2; wherein, the molar ratio of compound 1 to anhydrous methanol is 1: (10-90), further 1 : (80~90), further being 1:85; the first base is selected from anhydrous potassium carbonate, anhydrous sodium carbonate, anhydrous potassium acetate, anhydrous cesium carbonate, anhydrous sodium acetate, anhydrous potassium phosphate At least one, the molar ratio of compound 1 to the first base is 1: (0.3-4), further 1: (2.5-3) and further 1:3; the first organic solvent is selected from N-methylpyrrolidone (NMP ), toluene, N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide, the amount ratio of compound 1 to the first organic solvent is 1g: (8~ 15)ml, further 1g: 10mL; the rea...
Embodiment 1
[0053] Synthesis of 1,6-diMeOPDI:
[0054] (1) Add 1.2g of compound 1a and 600mg of anhydrous potassium carbonate into a microwave reaction flask, then add 5mL of anhydrous MeOH and 12mL of anhydrous NMP, heat to 100°C in a microwave reactor, and stop the reaction after 1h. The reactant was poured into 100mL dilute hydrochloric acid, the solid obtained by suction filtration was washed with water, dried and separated by column chromatography to obtain 423.4 mg of compound 2a (40% yield). The hydrogen spectrum and mass spectrum of compound 2a are shown in Figure 1~2 .
[0055] (2) Add compound 2a (320mg), palladium acetate (10mg), n-butyl bis (1-adamantyl) phosphine (32mg), anhydrous potassium carbonate (122mg), 7-tridecylamine in the autoclave (176mg) and toluene (15mL) were assembled into a reaction vessel, deoxygenated with nitrogen, and filled with 1MPa carbon monoxide gas, and the reactants were heated to 110°C for 3h. After the toluene was removed by the rotary evaporat...
Embodiment 2
[0059] Synthesis of 1,6-diHOPDI:
[0060] Add 80mg of 1,6-diMeOPDI to a 100ml two-necked bottle, pump nitrogen for 30min, add 5mL of dichloromethane to remove water and deoxygenate, lower it to 0°C and slowly add 0.3mL of boron tribromide in hexane alkane solution (1M), gradually warmed up to 25°C and stirred for 10 hours, slowly poured into 200mL of water after the reaction, extracted with dichloromethane, separated and purified the organic layer after drying to obtain purple red compound 4a (1,6-diHOPDI) (54 mg, 70%).
[0061] Concrete reaction formula is as follows:
[0062]
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