Benzoxanthene-containing compound material and application thereof
A technology of benzoxanthene and compounds, which is applied in the field of materials containing benzoxanthene compounds, can solve the problems of different performances, etc., and achieve the effects of simple and easy preparation methods, improved life attenuation, and improved life
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Embodiment 1
[0031] Embodiment 1: the synthesis of compound 1
[0032] Under the protection of nitrogen, add 500g of tetrahydrofuran and 50g of raw material A into the reaction bottle, drop the temperature to -95~-100°C, add 140ml of n-BuLi (n-butyllithium n-hexane solution) dropwise, keep it warm for 1h after dropping, and add 94g of raw material B into Dissolve in 940g of tetrahydrofuran, drop it into the reaction system, keep it warm for 3 hours after the drop, and then slowly drop the reaction solution into water for hydrolysis, then add 600g of toluene for extraction, wash with water three times to be close to neutral, then separate and recrystallize by column chromatography to obtain Intermediate C 89.2g, total yield 75%, liquid phase purity 99.5%.
[0033]
[0034] Under a nitrogen atmosphere, add 27g of raw material D-1 and 270g of dichloromethane into the reaction flask, then add 35.5g of boron trifluoride ether solution, dissolve 89g of intermediate C in 890g of dichloromethan...
Embodiment 2
[0037] Embodiment 2: the synthesis of compound 2
[0038]
[0039] Weigh compound D-3, intermediate 1 and t-BuONa (sodium tert-butoxide) according to the molar ratio 1:1.1:2, add catalyst Pd(OAc) 2 Palladium acetate and S-phos (2-dicyclohexylphosphine-2', 6'-dimethoxybiphenyl), the solvent is xylene, the solvent amount is 8 times the weight of compound D-3, and kept at 125°C After 8 hours of reaction, liquid phase detection showed that there was almost no intermediate 1 remaining, and the purity of the reaction liquid phase was 98.2%. Compound 2 was obtained after cooling, filtering, boiling, beating, and recrystallization, with a yield of 85.5% and a liquid phase purity of 99.3%.
[0040] Compound 2 NMR data: 1H NMR: δ7.20-7.45 (13H, 7.34, 7.27, 7.42, 7.22, 7.21, 7.28, 7.39, 7.31), 7.53-7.63 (3H, 7.62, 7.57), 7.66-7.76 (2H, 7.72, 7.73), 7.77-7.95(10H,7.83,7.81,7.84,7.84,7.89,7.90,7.91,7.95),7.96(1H),8.23(1H),8.51(1H).
Embodiment 3
[0041] Embodiment 3: the synthesis of compound 3
[0042]
[0043] Weigh compound D-4, intermediate 1 and t-BuONa (sodium tert-butoxide) according to molar ratio 1:1.1:2, add catalyst Pd (PPh 3 ) 2 Cl 2 (bis(triphenylphosphine)palladium dichloride) and X-phos(2-dicyclohexylphosphine-2',4',6'-triisopropylbiphenyl), the solvent is toluene, and the solvent amount is compound 10 times the weight of D-4, heat preservation reaction at 95° C. for 12 hours, liquid phase detection, the reaction purity is 98.2%. Compound 3 was obtained after cooling, filtering, boiling, beating, and recrystallization, with a yield of 75.5% and a liquid phase purity of 98.5%.
[0044] Compound 3 NMR data: 1 H NMR: δ7.20-7.52(16H,7.32,7.27,7.38,7.42,7.45,7.24,7.21,7.25,7.36,7.31),7.60(2H),7.76-7.94(10H,7.87,7.89,7.85,7.77 ,7.97,7.90,7.85),7.95(1H).
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