Method for preparing hydrazone compound
A technology of aldehyde compounds and compounds, applied in the preparation of hydrazones, organic chemistry and other directions, can solve problems such as hydrazone compounds that have not been disclosed
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Embodiment 1
[0031] Embodiment 1: Get the R base to be hydrogen, that is, the aldehyde compound is glyoxal, and the chemical formula is C 2 o 2 h 2 .
[0032] 1) Dissolving p-chlorophenylhydrazine hydrochloride in water, and extracting and removing polychlorinated biphenyls under the protection of an inert gas, to obtain a polychlorinated biphenyl-free aqueous solution of p-chlorophenylhydrazine hydrochloride;
[0033] 2) Mix glyoxal with deionized water to obtain an aqueous solution of glyoxal with a concentration of 0.5 mol / L;
[0034] 3) Add the p-chlorophenylhydrazine hydrochloride aqueous solution obtained in the above step 1) and the glyoxal aqueous solution prepared in the above step 2) into a reactor at the same time, and control the reaction temperature in the reactor to 25°C. The reaction pH value is PH5~6, and the adding speed of controlling the p-chlorophenylhydrazine hydrochloride aqueous solution is 0.1mol / min, and the adding speed of controlling the glyoxal aqueous soluti...
Embodiment 2
[0037] Example 2: Take the R group as a hydroxyl group (—OH), that is, the aldehyde compound is glyoxylic acid, and the chemical formula is CHOCO 2 H.
[0038] 1) Dissolve p-chlorophenylhydrazine hydrochloride in water, remove polychlorinated biphenyls under the protection of inert gas, and obtain a polychlorinated biphenyl-free aqueous solution of p-chlorophenylhydrazine hydrochloride;
[0039] 2) Mix glyoxylic acid with deionized water to obtain a glyoxylic acid aqueous solution with a concentration of 0.5mol / L;
[0040] 3) Add the p-chlorophenylhydrazine hydrochloride aqueous solution obtained in the above step 1) and the glyoxylic acid aqueous solution prepared in the above step 2) into a reactor at the same time, and control the reaction temperature in the reactor to 23-26 ℃, the reaction pH value is PH5~6, the adding rate of p-chlorophenylhydrazine hydrochloride aqueous solution is controlled to be 0.15mol / min, the adding rate of glyoxylic acid aqueous solution is contr...
Embodiment 3
[0043] Embodiment 3: get the R base to be an alkyl group (—CH 3 ), that is, the aldehyde compound is methylglyoxal, and its chemical formula is CH 3 COCHO.
[0044] 1) Dissolve p-chlorophenylhydrazine hydrochloride in water, remove polychlorinated biphenyls under the protection of inert gas, and obtain a polychlorinated biphenyl-free aqueous solution of p-chlorophenylhydrazine hydrochloride;
[0045] 2) Mix methylglyoxal with deionized water to obtain an aqueous solution of methylglyoxal with a concentration of 1 mol / L;
[0046]3) Add the p-chlorophenylhydrazine hydrochloride aqueous solution obtained in the above step 1) and the aceguvaldehyde aqueous solution prepared in the above step 2) into a reactor at the same time, and control the reaction temperature in the reactor to 26-30°C , the reaction pH value is PH5~6, and the adding speed of controlling p-chlorophenylhydrazine hydrochloride aqueous solution is 0.2mol / min, and the adding speed of controlling the methylglyoxal...
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