Beta-carboline derivative as well as preparation method and application thereof
A technology of derivatives and carbolines, which is applied in the field of β-carboline derivatives and its preparation, can solve the problems of reduced curative effect due to drug resistance, decreased therapeutic effect, and restrictions on long-term use, and achieves obvious anti-tumor effects, significant phototoxicity, and The effect of the novel mechanism of action
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Embodiment 1
[0265] The present embodiment is a preparation method of β-carboline derivatives, comprising the following steps:
[0266] S1. Preparation of compound 2:
[0267]
[0268] Tryptophan (compound 1, 0.82g, 4mmol) was dissolved in 20mL of methanol, and thionyl chloride (0.29mL, 4mmol) was added dropwise under ice-cooling, condensed and refluxed at 100°C for 7h, and the obtained solution was distilled off under reduced pressure to remove the solvent. After rinsing with ethyl acetate, suction filtration and drying, 0.98 g of white powder (compound 2) was obtained with a yield of 96.4%.
[0269] S2, preparation of compound 3:
[0270]
[0271] Add compound 2 (1.019g, 4mmol) to the reaction tube, then add benzaldehyde (408μL, 4mmol), dissolve in 15mL of isopropanol, heat and reflux at 90°C for 10h under the protection of argon, and distill off the solvent from the obtained liquid under reduced pressure , add benzene to stir, filter with suction, and dry to obtain 1.12 g of lig...
Embodiment 2
[0287] This embodiment is a preparation method of an iridium complex, comprising the following steps:
[0288] S1. Preparation of Compound 8:
[0289]
[0290] IrCl 3 ·nH 2 O (1.192g, 2mmol) and ppy (0.62g, 4mmol) were added to a mixed solution of ethylene glycol-ether and water (3:1, v / v) at a molar ratio of 1:2, heated to reflux for 24h, filtered, The crude product was passed through a silica gel column to obtain 0.90g Ir 2 (ppy) 4 Cl 2 (Compound 8), yield 84.0%.
[0291] S2. Preparation of compound 9:
[0292]
[0293] Ir 2 (ppy) 4 Cl 2 (Compound 8, 2.054g, 2mmol) and PPβC (Compound 7, 1.86g, 4mmol) were dissolved in the mixed solution of dichloromethane / methanol (2:1, v / v), refluxed for 4h under the protection of argon, and the reaction After the solution was cooled to room temperature, CH was removed by rotary evaporation. 2 Cl 2 After transferring to a beaker, 20 mL of KPF was added to the solution 6 saturated aqueous solution. After cooling overnight...
Embodiment 3
[0299] This embodiment is a preparation method of an iridium complex, comprising the following steps:
[0300] S1. Preparation of compound 10:
[0301]
[0302] IrCl 3 ·nH 2 O (1.192g, 2mmol) and dfppy (0.76g, 4mmol) were added to a mixed solution of ethylene glycol-ether and water (3:1, v / v) at a molar ratio of 1:2, heated to reflux for 24h, and filtered 0.91g Ir 2 (dfppy) 4 Cl 2 (Compound 10), yield 75.0%.
[0303] S2. Preparation of compound 11:
[0304]
[0305] Ir 2 (dfppy) 4 Cl 2 (2.432g, 2mmol) and compound 7 (1.86g, 4mmol) were dissolved in a mixed solution of dichloromethane / methanol (2:1, v / v), refluxed for 4h under the protection of argon, and the solution was cooled after the reaction to room temperature, rotary evaporation to remove CH 2 Cl 2 After transferring to a beaker, 20 mL of KPF was added to the solution 6 saturated aqueous solution. After cooling overnight at 4°C in the refrigerator, it was collected by filtration, dried in vacuo, and ...
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