How can I get rid of excess hydrazine hydrate 99%??
The reaction is converting an ester into hydrazide , required excess amount of HH to be done with ethanol as solvent.
I removed ethanol by RotaVap, but now My crude contain excess HH!
In this case, you supposed that the reaction was done 100%. But this is incorrect, and there is unreacted fraction of the ester that must also be removed. So, I recommend with utilizing Column Chromatography to separate the reaction mixture and obtain the product with high purity.
Regards.
HH can be decomposed (disproportionation) to NH3 and N2 by heating at 200-300 centigrade, but it's dangerous because of ignition. You could use ultra-disperse powders of Cu, Co, Ni, Ag due to their catalytic activity in this disproportionation, as a consequence, there's no need in heating and the products of that decomposition are N2 and H2. After the process has been done, you should wash you mixture out of this metallic powder. Although a don't know anything about interaction between these metals and hydrazides. Well, it'll be a good experiment! Good luck!
Well, it could be obvious but, did you try RotaVaping @60-70 °C? On the other hand, did you try to lyophilize the final crude? I think one of these two paths could help you. Good luck!
In this case, you supposed that the reaction was done 100%. But this is incorrect, and there is unreacted fraction of the ester that must also be removed. So, I recommend with utilizing Column Chromatography to separate the reaction mixture and obtain the product with high purity.
Regards.
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