Epoxy platinum complex and its preparation method and use
A technology of platinum complexes and epoxyplatinum, applied in the field of medicine, can solve problems such as systemic toxicity and harmful side effects
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Embodiment 1
[0083] Example 1 Preparation of 5-(4-hydroxyphenyl)thiophene-2-aldehyde
[0084]
[0085] 4-iodophenol (2.2g, 10mmol), 30ml of toluene and 30ml of ethanol were mixed, stirred at room temperature for 5 minutes, and then added 30ml of 2mol / L K 2 CO 3 The solution continued to be stirred evenly. Vacuum, replace nitrogen, repeat the operation 3 times, under nitrogen protection, add Pd (PPh 3 ) 4 (350 mg, 0.3 mmol) and 5-formyl-2-thiopheneboronic acid (1.87 g, 12 mmol), then the mixture was warmed to 85°C and stirring was continued for 8 hours. After the reaction was completed, the temperature was lowered to room temperature, and the solvent was spin-dried by a rotary evaporator, and then chromatographed on a silica gel column with dichloromethane:ethyl acetate=20:1 (V / V) as the eluent to obtain 920 mmg of yellow powder, with a yield of 920 mmg. 45%. 1 H NMR (300MHz, CDCl 3 )δ9.89(s,1H),δ7.74(d,1H,J=3.9Hz),δ7.61(m,2H),δ7.31(d,1H,J=3.9Hz),δ6.39 (m, 2H), δ 4.97 (s, 1H).
Embodiment 2
[0086] Preparation of Example 2 Ligand 3
[0087]
[0088] 5-(4-Hydroxyphenyl)thiophen-2-aldehyde (920 mmg, 4.5 mmol) was added to 200 mL of water, stirred, then o-aminothiophenol (1.25 g, 10 mmol) was added, and the temperature was raised to 110° C. to react for 3 hours. After cooling to room temperature, extract with ether, spin dry the solvent, and purify by silica gel column chromatography with dichloromethane as the eluent to obtain 900 mg of orange powder with a yield of 64%. 1 H NMR (300MHz, CDCl 3 )δ8.06(d,1H,J=8.1Hz),δ7.86(d,1H,J=7.8Hz),δ7.63(d,1H,J=4.2Hz),δ7.60(m,2H ),δ7.52(t,1H,J=7.2Hz),,δ7.41(t,1H,J=7.2Hz),δ7.25(d,1H,J=4.2Hz),δ6.93(m ,2H).ESI-HRMS([C17H11NOS2+H] + ): Calculated value 310.03, measured value 310.0335.
Embodiment 3
[0089] Example 3 Preparation of Ligand 4
[0090]
[0091] Ligand 3 (520 mg, 1.68 mmol) was stirred and dissolved in 15 mL of acetonitrile, evacuated, and replaced with nitrogen. After repeated operations 3 times, under nitrogen protection, sodium hydride (80 mmg, 2 mmol) was added, and then slowly added dropwise to the system. A dilute solution of 3-hydroxybenzyl bromide (628 mg, 3.36 mmol) in acetonitrile was added. After the dropwise addition, the temperature of the mixed solution was raised to 60° C. and the reaction was continued for 12 hours. After the reaction was completed, the temperature was lowered to room temperature, the solvent was spin-dried by a rotary evaporator, and then chromatographed on a silica gel column with dichloromethane as the eluent to obtain 100 mmg of yellow powder with a yield of 14%. 1 H NMR (300MHz, CDCl 3 )δ8.07(d,1H,J=8.1Hz),δ7.89(d,1H,J=7.8Hz),δ7.66(m,3H),δ7.52(t,1H,J=7.2Hz ),,δ7.41(t,1H,J=7.2Hz),δ7.29(m,3H),δ7.04(d,2H,J=6.6Hz),δ6.96(m...
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