Di(thiomethyl salicylate) di(o-chlorobenzyl) tin complex as well as preparation method and application
A technology of thiosalicylic acid and o-chlorobenzyl, applied in the field of complex preparation
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Embodiment 1
[0027] In a polytetrafluoroethylene microwave reaction tank, add 30 mL of methanol, 0.441 g (1 mmol) of bis(o-chlorobenzyl) tin dichloride, 0.308 g (2 mmol) of thiosalicylic acid, and 2 mmol of triethylamine. Seal it well and place it in a microwave reactor. The temperature of the microwave organic synthesis system was set at 120° C., and the reaction was irradiated with microwaves for 2 hours. Cool and filter to remove insoluble solids, remove part of the solvent by rotary evaporation of the filtrate, leave to precipitate a white solid, recrystallize from benzene to obtain 0.556 g of colorless crystal bis(methyl thiosalicylate) bis(o-chlorobenzyl)tin complex, Yield 79%, melting point: 142°C.
[0028] IR (KBr, cm -1 ): 3055.24, 2951.08ν(C-H), 1107.14ν(Sn-S), 476.41ν(Sn-C).
[0029] Elemental analysis (C 30 h 26 Cl 2 o 4 Sn), calculated (%): C, 51.16; H, 3.72. Found (%): C, 51.12; H, 3.79.
[0030] Crystallographic data: the crystal belongs to monoclinic crystal system...
Embodiment 2
[0032] In a polytetrafluoroethylene microwave reaction tank, add 30 mL of methanol, 0.440 g (1 mmol) of bis(o-chlorobenzyl) tin dichloride, 0.308 g (2 mmol) of thiosalicylic acid, and 2 mmol of triethylamine. Seal it well and place it in a microwave reactor. The temperature of the microwave organic synthesis system was set at 120° C., and the reaction was irradiated with microwaves for 2 hours. Cool and filter to remove insoluble solids, remove part of the solvent by rotary evaporation of the filtrate, leave to precipitate a white solid, recrystallize from benzene to obtain 0.555 g of colorless crystal bis(methyl thiosalicylate) bis(o-chlorobenzyl)tin complex, Yield 78%, melting point: 142°C.
[0033] IR (KBr, cm -1 ): 3055.24, 2951.08ν(C-H), 1107.14ν(Sn-S), 476.41ν(Sn-C).
[0034] Elemental analysis (C 30 h 26 Cl 2 o 4 Sn), calculated (%): C, 51.16; H, 3.72. Found (%): C, 51.12; H, 3.79.
[0035] Crystallographic data: the crystal belongs to monoclinic crystal system...
Embodiment 3
[0037] In a polytetrafluoroethylene microwave reaction tank, add 30 mL of methanol, 0.443 g (1 mmol) of bis(o-chlorobenzyl) tin dichloride, 0.308 g (2 mmol) of thiosalicylic acid and 2 mmol of triethylamine, and cover the Seal it well and place it in a microwave reactor. The temperature of the microwave organic synthesis system was set at 120° C., and the reaction was irradiated with microwaves for 2 hours. Cool and filter to remove insoluble solids, remove part of the solvent by rotary evaporation of the filtrate, leave to precipitate a white solid, recrystallize from benzene to obtain 0.556 g of colorless crystal bis(methyl thiosalicylate) bis(o-chlorobenzyl)tin complex, Yield 80%, melting point: 143°C.
[0038] IR (KBr, cm -1 ): 3055.24, 2951.08ν(C-H), 1107.14ν(Sn-S), 476.41ν(Sn-C).
[0039] Elemental analysis (C 30 h 26 Cl 2 o 4 Sn), calculated (%): C, 51.16; H, 3.72. Found (%): C, 51.12; H, 3.79.
[0040] Crystallographic data: the crystal belongs to monoclinic cry...
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