Organic compound and electrochromic element
一种有机化合物、电致变色的技术，应用在有机化学、变色荧光材料、周期表第5/15族元素的化合物等方向，能够解决化合物不充分等问题
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Embodiment 1
[0093] Embodiment 1 (synthesis of exemplary compound A-3)
[0094]
[0095] Tetrahydrofuran (80ml) and diisopropylamine (16ml, 110mmol) were added to the reactor, and the mixture was cooled to -70°C. After gradually dropping a 1.6M butyllithium hexane solution (70ml, 110mmol) into the solution, the temperature was raised to 0C to prepare an LDA solution. Separately, N,N-diethylnicotinamide (18 g, 100 mmol), triisopropyl borate (25 ml, 110 mmol) and tetrahydrofuran (80 ml) were prepared, and the mixture was cooled to -10°C. After the pre-prepared LDA solution was gradually dropped into the solution and the solution was stirred at room temperature for 2 hours, [1,1'-bis(diphenylphosphino)ferrocene]palladium(II) dichloride was added thereto ) dichloromethane adduct (1.7g, 2mmol), 4-bromoquinoline (13.7g, 66mmol), tetrahydrofuran (160ml), potassium phosphate (139g, 250mmol) and water (150ml), and the solution at 60 Stir at °C for 14 hours. After the reaction solution was lef...
Embodiment 2
[0102] Embodiment 2 (synthesis of exemplary compound A-2)
[0103] Exemplary compound A-3 (210 mg, 0.3 mmol) was dissolved in water. A solution in which 500 mg of potassium hexafluorophosphate was dissolved was added dropwise, and the solution was stirred at room temperature for 3 hours. The precipitated crystals were filtered off and washed sequentially with isopropanol and diethyl ether to obtain 212 mg of Exemplified Compound A-2 (yield: 96%).
[0104] The structure of Compound A-2 was confirmed by NMR measurement. 1 H NMR(DMSO-d6,500MHz), σ(ppm): 10.22(s,1H),9.81(s,1H),9.48(d,1H),9.41(d,1H),9.31(d,1H), 8.82 (d,1H),8.40(t,1H),8.27(t,1H),5.17(t,2H),4.74(t,2H),2.06(m,4H),1.79(s,6H),1.50 -1.22(m,16H),0.87(m,6H).
Embodiment 3
[0105] Example 3 (production of electrochromic element and evaluation of characteristics)
[0106] Tetrabutylammonium perchlorate as an electrolyte was dissolved in propylene carbonate at a concentration of 0.1 M, and then the exemplary compound A-2 of Example 2 was dissolved at a concentration of 40.0 mM to obtain an EC medium. Next, insulating layers (SiO 2 ). A PET film (Teijin DuPont Films Japan Limited, Melinex (registered trademark) S, 125 μm thick) for defining the distance between the substrates was arranged between a pair of glass substrates with transparent electrode films. Then, except for the injection port for injecting the EC medium, the substrate and the PET film were bonded and sealed by an epoxy-based adhesive. A cell with an injection port is fabricated as described above. Next, after injecting the EC medium obtained in the above method by vacuum injection, the injection port was sealed with an epoxy-based adhesive to obtain an EC element.
[0107]The EC ...
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