A kind of di-n-butyltin complex and its preparation method and application
A technology of di-n-butyl tin and di-n-butyl tin oxide is applied in the directions of tin organic compounds, pharmaceutical formulations, organic chemical methods, etc., can solve problems such as undiscovered compounds, and achieves simple preparation method, low cost, and good anticancer activity. Effect
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Embodiment 1
[0042] Preparation of 2-carbonyl-3-phenylpropionic acid p-methylbenzoylhydrazone di-n-butyltin complex:
[0043] Add 0.249g (1.0mmol) di-n-butyltin oxide, 0.150g (1.0mmol) p-toluylhydrazide, 0.205g (1.1mmol) sodium phenylpyruvate and 15mL solvent in a 100mL three-necked flask protected by nitrogen Anhydrous methanol, react at 45~65°C for 8 hours, cool, filter, and control solvent volatilization and crystallization at 20~35°C to obtain yellow transparent crystals, namely 2-carbonyl-3-phenyl p-toluylhydrazone di-n-butyltin propionate complex. Yield: 85.5%. Melting point: 97~99°C (dec).
[0044] Elemental analysis (C 52 h 72 N 4 o 8 sn 2 ): Calculated: C 55.84, H 6.49, N 5.01; Found: C 55.90, H 6.45, N 5.00.
[0045] FT-IR (KBr, ν / cm -1 ): 3421, 3030, 2956, 2924, 2856, 1606, 1585, 1490, 1394, 1338, 1300, 1178, 1062, 1022, 918, 960, 837, 750, 707, 623, 588, 5455, 6.45
[0046] 1 H NMR (500 MHz, CDCl 3 , δ / ppm): 8.14 (d, J =8.1 Hz, 2H), 7.54 (d, J =7.0 Hz, 2H), 7....
Embodiment 2
[0051] Preparation of 2-carbonyl-3-phenylpropionic acid p-methylbenzoylhydrazone di-n-butyltin complex:
[0052] Add 0.248g (1.0mmol) di-n-butyltin oxide, 0.150g (1.0mmol) p-toluylhydrazide, 0.195g (1.05mmol) sodium phenylpyruvate and 35mL solvent in a 100mL three-necked flask protected by nitrogen Anhydrous methanol, react for 5 hours at a temperature of 45~65°C, cool, filter, and control solvent volatilization and crystallization at a temperature of 20~35°C to obtain a yellow transparent crystal, which is 2-carbonyl-3-phenyl p-toluylhydrazone di-n-butyltin propionate complex. Yield: 87.5%. Melting point: 97~99°C (dec).
[0053] Elemental analysis (C 52 h 72 N 4 o 8 sn 2 ): Calculated: C 55.84, H 6.49, N 5.01; Found: C 55.90, H 6.45, N 5.00.
[0054] FT-IR (KBr, ν / cm -1 ): 3421, 3030, 2956, 2924, 2856, 1606, 1585, 1490, 1394, 1338, 1300, 1178, 1062, 1022, 918, 960, 837, 750, 707, 623, 588, 5455, 6.45
[0055] 1 H NMR (500 MHz, CDCl 3 , δ / ppm): 8.14 (d, J =8.1 H...
Embodiment 3
[0060] Preparation of 2-carbonyl-3-phenylpropionic acid p-methylbenzoylhydrazone di-n-butyltin complex:
[0061] Add 0.248g (1.0mmol) di-n-butyltin oxide, 0.158g (1.05mmol) p-toluylhydrazide, 0.214g (1.15mmol) sodium phenylpyruvate and 25mL solvent in a 100mL three-necked flask protected by nitrogen Anhydrous methanol, react for 24 hours at a temperature of 45~65°C, cool, filter, and control solvent volatilization and crystallization at a temperature of 20~35°C to obtain a yellow transparent crystal, which is 2-carbonyl-3-phenyl p-toluylhydrazone di-n-butyltin propionate complex. Yield: 88.8%. Melting point: 97~99°C (dec).
[0062] Elemental analysis (C 52 h 72 N 4 o 8 sn 2 ): Calculated: C 55.84, H 6.49, N 5.01; Found: C 55.90, H 6.45, N 5.00.
[0063] FT-IR (KBr, ν / cm -1 ): 3421, 3030, 2956, 2924, 2856, 1606, 1585, 1490, 1394, 1338, 1300, 1178, 1062, 1022, 918, 960, 837, 750, 707, 623, 588, 5455, 6.45
[0064] 1 H NMR (500 MHz, CDCl 3 , δ / ppm): 8.14 (d, J =8.1 H...
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