Cyclometalated ruthenium complex as well as synthetic method and application thereof
A technology of ruthenium complexes and cyclometallation, which is applied in the synthesis of cyclometallated ruthenium complexes, and in the field of cyclometallated ruthenium complexes, can solve problems such as drug failure, cumulative drug resistance of tumor cells, and reduced tumor cell killing effect
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Embodiment 1
[0099] Synthesis of Cyclometallated Ruthenium Complexes Ru1
[0100] ①Synthesis of N-Ts-β-phenylethylamine
[0101] Dissolve phenethylamine (12.1g, 100mmol) and triethylamine (30.3g, 300mmol) in 85ml of dichloromethane, then slowly add p-toluenesulfonyl chloride (18.05g, 95mmol) at -15°C, drop After the addition, remove the freezer, return to room temperature (25°C), stir for 6 hours, TLC detects that the raw material point disappears (phenethylamine), indicating that the reaction is complete; then, add 100ml of water to wash, and wash with 25ml of 1M HCl solution until the solution is weakly acidic , and the solvent was spin-dried to obtain an oil, which was dissolved by adding 10ml of ethanol and dissolved in a hot water bath at 70°C; then adding 50ml of water, stirring, and a white precipitate was precipitated, put it in a refrigerator at 4°C, and filtered with suction to obtain N-Ts-β-phenethylamine, the yield is 90%.
Embodiment 2
[0111] Synthesis of Cyclometallated Ruthenium Complexes Ru2
[0112] ①Synthesis of N-Ts-β-phenylethylamine
[0113] Dissolve phenethylamine (12.1g, 100mmol) and triethylamine (30.3g, 300mmol) in 80ml of dichloromethane, then slowly add p-toluenesulfonyl chloride (18.05g, 95mmol) at -10°C, drop After the addition, remove the freezer, return to room temperature (25°C), stir for 5 hours, TLC detects that the raw material point disappears (phenethylamine), indicating that the reaction is complete; then, add 100ml of water to wash, and wash with 25ml of 1M HCl solution until the solution is weakly acidic , and the solvent was spin-dried to obtain an oil, which was dissolved by adding 10ml of ethanol and dissolved in a hot water bath at 70°C; then adding 50ml of water, stirring, and a white precipitate was precipitated, put it in a refrigerator at 4°C, and filtered with suction to obtain N-Ts-β-phenethylamine, the yield is 88%.
[0114] ② 1-p-tolyl-2-tosyl-1,2,3,4-tetrahydroisoqui...
Embodiment 3
[0123] Synthesis of Cyclometallated Ruthenium Complexes Ru3
[0124] ①Synthesis of N-Ts-β-phenylethylamine
[0125] Dissolve phenethylamine (12.1g, 100mmol) and triethylamine (30.3g, 300mmol) in 80ml of dichloromethane, then slowly add p-toluenesulfonyl chloride (18.05g, 95mmol) at -8°C, drop After the addition, remove the freezer, return to room temperature (25°C), stir for 4 hours, TLC detects that the raw material point disappears (phenethylamine), indicating that the reaction is complete; then, add 120ml of water to wash, and wash with 25ml of 1M HCl solution until the solution is weakly acidic , and the solvent was spin-dried to obtain an oil, which was dissolved by adding 12ml of ethanol and dissolved in a hot water bath at 70°C; then adding 50ml of water, stirring, and a white precipitate was precipitated, put it in a refrigerator at 3°C, and filtered with suction to obtain N-Ts-β-phenylethylamine, the yield is 92%.
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