2-oxo-butyric acid p-methyl benzoyl hydrazone di-n-butyl tin complex and preparation method and application thereof
A technology of nitrobenzoylhydrazone di-n-butyltin and di-n-butyltin oxide, which is applied in tin organic compounds, pharmaceutical formulations, organic chemical methods, etc., can solve the problems of undiscovered compounds and achieve simple and good preparation methods Anticancer activity, low-cost effect
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Embodiment 1
[0042] Preparation of 2-carbonylbutanoic acid p-nitrobenzoylhydrazone di-n-butyltin complex:
[0043] Add 0.249g (1.0mmol) di-n-butyltin oxide, 0.181g (1.0mmol) p-nitrobenzohydrazide, 0.112g (1.1mmol) 2-butanone acid and 15mL The solvent is anhydrous methanol, react at a temperature of 45~65°C for 8 hours, cool, filter, and control the solvent volatilization and crystallization at a temperature of 20~35°C to obtain a yellow transparent crystal, which is 2-carbonylbutyric acid p-nitrate Di-n-butyltin complexes of benzoylhydrazone. Yield: 81.9%. Melting point: 80~82°C (dec).
[0044] Elemental analysis (C 40 h 62 N 6 o 12 sn 2 ): Calculated: C 45.48, H 5.92, N 7.96; Found: C 45.54, H 6.00, N 7.95.
[0045] FT-IR (KBr, ν / cm -1 ): 3423, 2956, 2927, 2858, 1635, 1612, 1533, 1502, 1386, 1336, 1261, 1195, 1155, 1056, 1012, 966, 854, 806, 719, 684, 601, 5480, 25, 25 443, 422.
[0046] 1 H NMR (500 MHz, CDCl 3 , δ / ppm): 8.38 (d, J =9.0 Hz, 2H), 8.30 (d, J =9.0 Hz, 2H), ...
Embodiment 2
[0051] Preparation of 2-carbonylbutanoic acid p-nitrobenzoylhydrazone di-n-butyltin complex:
[0052] Add 0.249g (1.0mmol) di-n-butyltin oxide, 0.190g (1.0mmol) p-nitrobenzohydrazide, 0.107g (1.05mmol) 2-butanone acid and 35mL Solvent anhydrous methanol, react for 5 hours at a temperature of 45~65°C, cool, filter, and control the solvent volatilization and crystallization at a temperature of 20~35°C to obtain a yellow transparent crystal, which is 2-carbonylbutanoic acid p-nitrate Di-n-butyltin complexes of benzoylhydrazone. Yield: 85.5%. Melting point: 80~82°C (dec).
[0053] Elemental analysis (C 40 h 62 N 6 o 12 sn 2 ): Calculated: C 45.48, H 5.92, N 7.96; Found: C 45.54, H 6.00, N 7.95.
[0054] FT-IR (KBr, ν / cm -1 ): 3423, 2956, 2927, 2858, 1635, 1612, 1533, 1502, 1386, 1336, 1261, 1195, 1155, 1056, 1012, 966, 854, 806, 719, 684, 601, 5480, 25, 25 443, 422.
[0055] 1 H NMR (500 MHz, CDCl 3 , δ / ppm): 8.38 (d, J =9.0 Hz, 2H), 8.30 (d, J =9.0 Hz, 2H), 3.49 ...
Embodiment 3
[0060] Preparation of 2-carbonylbutanoic acid p-nitrobenzoylhydrazone di-n-butyltin complex:
[0061] Add 0.249g (1.0mmol) di-n-butyltin oxide, 0.190g (1.05mmol) p-nitrobenzohydrazide, 0.117g (1.15mmol) 2-butanonic acid and 25mL The solvent is anhydrous methanol, reacted for 24 hours at a temperature of 45~65°C, cooled, filtered, controlled solvent volatilization and crystallization at a temperature of 20~35°C, and obtained yellow transparent crystals, namely 2-carbonylbutanoic acid p-nitrate Di-n-butyltin complexes of benzoylhydrazone. Yield: 83.6%. Melting point: 80~82°C (dec).
[0062] Elemental analysis (C 40 h 62 N 6 o 12 sn 2 ): Calculated: C 45.48, H 5.92, N 7.96; Found: C 45.54, H 6.00, N 7.95.
[0063] FT-IR (KBr, ν / cm -1 ): 3423, 2956, 2927, 2858, 1635, 1612, 1533, 1502, 1386, 1336, 1261, 1195, 1155, 1056, 1012, 966, 854, 806, 719, 684, 601, 5480, 25, 25 443, 422.
[0064] 1 H NMR (500 MHz, CDCl 3, δ / ppm): 8.38 (d, J =9.0 Hz, 2H), 8.30 (d, J =9.0 Hz,...
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