Tin complex with 2-acetyl pyridine thiosemicarbazone as ligand and synthesis method thereof
A technology of acetylpyridine thiosemicarbazide and synthesis method, which is applied in the directions of tin organic compounds, compounds of elements of Group 4/14 of the periodic table, chemical instruments and methods, etc., to achieve the effect of strong antitumor activity and enhanced activity
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Embodiment 1
[0028] The synthesis of C1 tin complexes, the concrete synthesis method is:
[0029] (1) Dissolve 3mmol of 4-methylthiosemicarbazide in 25ml of methanol, then add 3mmol of 2-acetylpyridine, add dropwise 1ml of acetic acid, mix well; reflux at 65°C for 8h, filter, and the filtrate is volatile at room temperature, with a white color Crystals were precipitated; filtered and washed three times with absolute ethanol to obtain ligand L1 (yield; 89.12%, white crystals);
[0030] Yield: 89.12%, C 9 h 12 N 4 S: C, 51.90; H, 5.81; N, 26.90; S, 15.39. Found: C, 51.91; H, 5.83; N, 26.89; (s,NH),3043(m,aromatichydrogen),1579(m),1494(s),1474(s,aromatic),1364(m,C=N),1286(s,thioamide),1148(s) ,1073(s),905(m,C-H),741(m,C=S),570(m);
[0031] (2) Dissolve the ligand L1 (0.1mmol) obtained in step (1) in 10ml methanol, reflux at 65°C for 4h, add SnCl 2 (0.1mmol) filter after stirring at room temperature for 4h, after the filtrate is divided into three parts on average, add methanol and ethan...
Embodiment 2
[0034] The synthesis of C2 tin complexes, the concrete synthesis method is:
[0035] (1) Dissolve 3mmol of 4,4-dimethylthiosemicarbazide in 25ml of methanol, then add 3mmol of 2-acetylpyridine, dropwise add 1ml of acetic acid, mix well; reflux at 65°C for 8h, filter, and concentrate under reduced pressure after the reaction , extracted with ethyl acetate, washed successively with saturated sodium bicarbonate and water, and separated by silica gel column chromatography (petroleum ether: ethyl acetate volume ratio = 10:1) to obtain ligand L2 (89.31%, pale yellow solid);
[0036] Yield: 89.31%, C 10 h 14 N 4 S: C, 54.03; H, 6.35; N, 25.20; S, 14.42. Found: C, 54.02; H, 6.34; N, 25.22; (s,NH),3094(m,aromatichydrogen),1580(m),1497(s),1461(s,aromatic),1378(m,C=N),1285(s,thioamide),1146(s) ,1093(s),889(m,C-H),736(m,C=S),586(m);
[0037] (2) Dissolve the ligand L2 (0.1mmol) obtained in step (1) in 15ml methanol, reflux at 65°C for 4h, add SnCl 2 (0.1mmol) filter after stirring a...
Embodiment 3
[0040] The synthesis of C3 tin complexes, the concrete synthesis method is:
[0041] (1) Dissolve 3mmol of 3-pyrrole thiosemicarbazide in 20ml of methanol, add 3mmol of 2-acetylpyridine, dropwise add 0.8ml of acetic acid, mix well; reflux at 65°C for 8h, filter, put the filtrate in a fume hood, Slowly volatilized until pale yellow crystals were precipitated; washed three times with absolute ethanol to obtain ligand L3 (yield; 88.54%, pale yellow crystals);
[0042] Yield: 88.54%, C 12 h 16 N 4 S: C, 58.04; H, 6.49; N, 22.56; S, 12.91. Found: C, 58.08; H, 6.47; N, 22.54; (s,NH),2971(m,aromatichydrogen),1584(m),1534(s),1416(s,aromatic),1338(m,C=N),1288(s,thioamide),1163(s) ,1047(s),899(m,C-H),720(m,C=S),600(m);
[0043] (2) Dissolve the ligand L3 (0.1mmol) obtained in step (1) in 15ml methanol, reflux at 65°C for 4h, add SnCl 2 (0.1mmol) filter after stirring at room temperature for 4h, after the filtrate is divided into three parts on average, add methanol and ethanol res...
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