Synthesis of mononuclear (polynuclear) complex of Schiff's base and bismuth
A Schiff base and nuclear coordination technology, applied in bismuth organic compounds, organic chemistry and other directions, can solve the problems of lack of systematic theoretical support, lack of high efficiency and low toxicity, lack of new methods and ideas for screening antibacterial and antitumor Simple, mild effects
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Embodiment 1
[0025] Example 1 Synthesis of o-vanillin ethylenediamine Schiff base and bismuth single (double) nuclear complex
[0026] (1) Preparation of o-vanillin ethylenediamine Schiff base. Add o-vanillin (2mmol, 0.304g) and ethylenediamine (1mmol, 0.12g) to 30ml of ethanol (50ml round bottom flask) respectively, stir at room temperature, and a yellow precipitate precipitates out. After reacting for 2 hours, filter, wash the filter cake with absolute ethanol, and dry to obtain o-vanillin ethylenediamine Schiff base with a yield of 64%. IR(KBr):v(cm -1 ): 3380.4, 2898.8, 2848.5, 1632.9, 1471.12, 1251.6, 1081.8. 1 H NMR (DMSO-d 6 , 400MHz): δ12.98(s, 2H), 8.92(s, 2H), 6.89~7.24(m, 6H), 4.00(s, 4H), 3.73(s, 6H). 13 C NMR (DMSO-d 6 , 400MHz): δ162, 152.9, 150.9, 125.1, 122.5, 122.1, 117.9, 68.7, 56.2.MS (EI): m / z328 (M + ).
[0027] (2) Synthesis of mononuclear complexes of o-vanillin ethylenediamine Schiff base and bismuth. Dissolve o-vanillin ethylenediamine Schiff's base (0.8mmo...
Embodiment 2
[0031] Example 2 Synthesis of o-vanillin condensed o-phenylenediamine Schiff base and bismuth single (double) nuclear complex
[0032] (1) Preparation of o-phenylenediamine Schiff base with o-vanillin. Add o-vanillin (2mmol, 0.304g) into 30ml of ethanol (100ml round bottom flask), heat in a water bath and stir to make it all dissolve. At the same time, pour the weighed o-phenylenediamine (1mmol, 0.108g) into a clean small beaker, add 20ml of ethanol, heat slightly and stir to make it all dissolve. The ethanol solution of o-phenylenediamine was slowly added dropwise to the o-vanillin solution to obtain an orange solution. After about 5 minutes, an orange crystalline solid precipitated out of the flask. The reaction was continued for another 1 h, and the reaction solution was transferred to a clean beaker. Cooling with an ice-water bath, more solids precipitated. Filtrate immediately to obtain an orange crystalline solid, which is washed and dried to obtain an orange o-vanilli...
Embodiment 3
[0037] Example 3 Synthesis of polynuclear complexes of o-vanillin ethylenediamine Schiff base and bismuth. Dissolve o-vanillin ethylenediamine Schiff base (0.4mmol, 0.1312g) in 25ml of methanol (50ml round bottom flask), heat and stir to dissolve the Schiff base to obtain a yellow transparent solution. Mix and grind bismuth nitrate (0.4mmol, 0.194g) and mannitol (0.4mmol, 0.0728g) into a paste, add 3ml of water, grind to obtain a clear solution, and then add 5ml of methanol. Slowly add the bismuth chelating agent solution dropwise into the methanol solution of Schiff's base to obtain a light yellow clear solution. When about 3 / 4 of the chelating agent is added, it tends to become turbid. Stop adding the chelating agent and continue heating and stirring. After 1h, transfer the solution in the flask to a beaker, let it stand still, and volatilize naturally. After 12h, a pale yellow granular precipitate precipitated out, washed and dried. A pale yellow granular solid was obtaine...
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