Method for preparing aldehyde semicarbazone Schiff base
A technology of semicarbazide and semicarbazide hydrochloride, applied in the direction of organic chemistry and the like, can solve the problems of serious environmental pollution, low yield and high energy consumption, and achieve the effects of low reaction temperature, high yield and simple operation
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Embodiment 1
[0027] 1) Add 1mol aldehyde (R=H), 1mol semicarbazide hydrochloride and 0.1mol p-aminobenzenesulfonic acid to a dry mortar, grind at room temperature, mix the raw materials evenly, and react the raw materials, grind until the reaction is complete The time required for completeness is 20 minutes. At this time, TLC detection found that the raw material point of aldehyde disappeared, and the developer of TLC was a mixed solvent of ethyl acetate and petroleum ether with a volume ratio of 1:3;
[0028] 2) Put the mortar in an oven and keep it warm at 80°C for 30 minutes; then cool to room temperature, wash with absolute ethanol, filter under reduced pressure, and concentrate the filtrate to dryness to obtain the target product 2-methyleneamino urea. Its yield reaches more than 95%, and its structural formula is:
[0029]
[0030] M.p. (melting point) = 120 ~ 123 ° C; IR (KBr, ν / cm -1 ): 3458.23, 3065.38, 1648.10, 1624.33, 993.28.
Embodiment 2
[0032] 1) Add 1mol aldehyde (R=CH 3 ), 1mol semicarbazide hydrochloride and 0.2mol p-aminobenzenesulfonic acid were ground at room temperature to mix the raw materials evenly and react the raw materials. The time required for grinding until the reaction was complete was 12 minutes. At this time, TLC detection found that the aldehyde The raw material point disappears, and the developer of TLC is a mixed solvent of ethyl acetate and petroleum ether with a volume ratio of 1:3;
[0033] 2) Put the mortar in an oven and keep it warm at 85°C for 50 minutes; then cool to room temperature, wash with absolute ethanol, filter under reduced pressure, and concentrate the filtrate to dryness to obtain the target product 2-ethyleneamino urea. Its yield reaches more than 95%, and its structural formula is:
[0034]
[0035] M.p.=175~176℃; IR (KBr, ν / cm -1 ): 3412.47, 3283.62, 3121.83, 1679.49, 402.71, 325.25.
Embodiment 3
[0037] 1) Add 1 mol of aldehyde (R=phenyl), 1.1 mol of semicarbazide hydrochloride and 0.2 mol of p-aminobenzenesulfonic acid to a dry mortar, grind at room temperature, mix the raw materials evenly, and react the raw materials, and grind until The time required for the reaction to complete is 10min. At this time, TLC detection found that the raw material point of aldehyde disappeared, and the developing agent of TLC was a mixed solvent of ethyl acetate and sherwood oil with a volume ratio of 1:3;
[0038] 2) Put the mortar in an oven and keep it warm at 80°C for 60 minutes; then cool to room temperature, wash with absolute ethanol, filter under reduced pressure, and concentrate the filtrate to dryness to obtain the target product 2-(phenylene methyl)-semicarbazide. Its yield reaches more than 95%, and its structural formula is:
[0039]
[0040] M.p.=220~222℃; IR (KBr, ν / cm -1 ): 3401.89, 3298.90, 3059.38, 1689.42, 603.71, 758.08, 689.40.
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