(All manipulations are under glovebox system)
In my reaction, there's Sodiumamide(NaNH2) as an impurity.
(sodium isopropylcyclopentadienide+ tetrakis(dimethylamido)zirconium)
I want to remove this impurity perfectly because there's only one impurity.
but the problem is if I distill the product it starts to decompose.
(schlenk technique, distilled under vacuum start 50-150℃, all-temperature decomposed. distilled outside with senior. vacuum at room temperature was okay. TGA finished at 300℃)
So I filter it with celite to filter but still little amount of Sodiumamide left.
If I filter it with celite, it decreases but this method is not good though.
Hi Jessica so-hee Choi, I assume that your target product is (C5H4iPr)Zr(NMe2)3. Is that correct? In that case you should do an extraction step first. You could use e.g. diethyl ether, n-pentane or toluene to extract the zirconium complex. Sodium amide is insoluble in these solvents. Thus it should be possible to remove the NaNH2 by filtration using Celite. The Celite layer can then be washed with the same solvent. After evaporation of the filtrate to dryness you can do the vacuum distillation.
Jessica so-hee Choi meanwhile your question is some time ago. Can you perhaps tell us if you have been successful isolating your zirconium complex?
Frank T. Edelmann So sorry for late comment. Actually I used toluene as you mentioned and succeed to remove the impurity. Product strongly combined to impurity so it was not easy to remove but it really works well. Thank you for your help so much and sorry for late mention.
Dear Jessica so-hee Choi many thanks for the udate. No need to be sorry. I'm just glad to hear hat the suggested procedure was successful. Good luck with your further research!