Preparation method for 2-substituted benzldehyde shrank hydrazine-sulfo-benzyl formate schiff base zinc and nickel complex
A technology of formaldehyde hydrazide benzyl dithiocarbamate and Schiff base, which is applied in the directions of drug combination, organic chemistry, antitumor drug and the like, and achieves the effects of simple and feasible preparation method, convenient industrial production, and easily available and cheap raw materials
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Embodiment 1
[0020] Example 1: Preparation of 2-chlorobenzaldehyde hydrazinyl dithioformate benzyl Schiff base zinc complex
[0021]
[0022] 1. In a 100mL round bottom flask, dissolve benzyl hydrazinodithioformate (1.98 g, 10.0 mmol) in 30 ml of absolute ethanol, and slowly add an equivalent amount of 2-chloro ethanol solution of benzaldehyde. Then after heating to reflux for 4h, cool to 0 o C, filter under reduced pressure, wash with ethanol, obtain pale yellow solid, dissolve the obtained solid in dehydrated alcohol and recrystallize and purify, obtain 2-chlorobenzaldehyde hydrazide dithioformic acid benzyl ester (H 2 L). Yield 57%. Anal. Calc. for C 15 h 13 ClN 2 S 2 : C, 56.2; H, 4.1; N, 8.7,Found: C, 55.8; H, 4.0; N, 8.9%.
[0023] 2. Dissolve 2-chlorobenzaldehyde hydrazinyl benzyl dithiocarbamate (0.32 g, 1.0 mmol) in 20 ml of absolute ethanol solvent, and add Zn(OAc) under stirring 2 2H 2 O (0.11 g, 0.5 mmol) in absolute ethanol was stirred and reacted for 4 hours, and...
Embodiment 2
[0024] Example 2: Preparation of 2-chlorobenzaldehyde hydrazinyl dithioformate benzyl Schiff base nickel complex
[0025]
[0026] The preparation method is the same as in Example 1. Nickel acetate was used instead of zinc acetate to obtain purple crystals with a yield of 56%. Anal. Calc. for C 30 h 24 Cl 2 N 4 S 4 Ni: C, 51.6; H, 3.5; N, 8.0. Found: C, 51.4; H, 3.3; N, 8.3%. See its crystal structure figure 2 , the crystallographic data are shown in Table 2, and the main bond lengths and bond angles are shown in Table 3.
Embodiment 3
[0027] Example 3: Preparation of 2-nitrobenzaldehyde hydrazinyl dithioformate benzyl Schiff base nickel complex
[0028]
[0029] The preparation method is the same as in Example 1. 2-nitrobenzaldehyde was substituted for 2-chlorobenzaldehyde, and nickel acetate was substituted for zinc acetate to obtain purple crystals with a yield of 56%. Anal. Calc. for C 30 h 24 N 6 o 4 S 4 Ni: C, 50.1; H, 3.4; N, 11.7. Found: C, 49.4; H, 3.3; N, 11.8%. See its crystal structure image 3 , the crystallographic data are shown in Table 2, and the main bond lengths and bond angles are shown in Table 3.
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