A kind of benzoxanthene compound material and its application
A technology for benzoxanthene and compound, which is applied in the field of benzoxanthene compound materials, can solve problems such as different performances, and achieves the effects of simple and easy preparation method, high yield and improved lifespan
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Embodiment 1
[0031] Example 1: Synthesis of Compound 1
[0032] Under nitrogen protection, 500 g of tetrahydrofuran and 50 g of raw material A were added to the reaction flask, the temperature was lowered to -95~-100 ℃, and 140 ml of n-BuLi (n-butyl lithium n-hexane solution) was added dropwise. In 940g tetrahydrofuran, it was dissolved and dropped into the reaction system. After the dropping was completed, it was incubated for 3h and the reaction was completed. After that, the reaction solution was slowly dropped into water for hydrolysis, and then 600g of toluene was added for extraction. Intermediate C 89.2 g, the total yield is 75%, and the liquid phase purity is 99.5%.
[0033]
[0034] Under nitrogen atmosphere, 27g of raw material D-1 and 270g of dichloromethane were added to the reaction flask, then 35.5g of boron trifluoride ether solution was added, 89g of intermediate C was dissolved in 890g of dichloromethane, and the temperature was lowered to -15~- The dichloromethane sol...
Embodiment 2
[0037] Example 2: Synthesis of Compound 2
[0038]
[0039] Weigh compound D-3, intermediate 1 and t-BuONa (sodium tert-butoxide) according to the molar ratio of 1:1.1:2, and 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 the temperature is kept at 125 ° C After the reaction for 8 hours, the liquid phase detection showed that there was basically no remaining intermediate 1, and the liquid phase purity of the reaction was 98.2%. Compound 2 was obtained through cooling, filtration, boiling, beating and recrystallization. The yield was 85.5%, and the liquid phase purity was 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] Example 3: Synthesis of Compound 3
[0042]
[0043] Weigh compound D-4, intermediate 1 and t-BuONa (sodium tert-butoxide) according to the molar ratio of 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 the compound 10 times the weight of D-4, the reaction was incubated at 95° C. for 12 hours, and the liquid phase detection showed that the reaction purity was 98.2%. Compound 3 was obtained through cooling, filtration, boiling, beating and recrystallization. The yield was 75.5%, and the liquid phase purity was 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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