Polymorphism Control of a Schiff base via solvent-free and solution based synthesis Marija Zbačnik ab , Ivana Nogalo a and Dominik Cinčić a Laboratory of General and Inorganic Chemistry, Department of Chemistry, University of Zagreb, Zagreb, Croatia 10002, E-mail: mzbacnik@chem.pmf.hr. b Department of Chemistry, University of the Free State, Bloemfontein 9300, South Africa, E-mail: ZbacnikM@ufs.ac.za
Polymorphism Control of a Schiff base via solvent-free and solution based synthesis Marija Zbačnik , Ivana Nogalo and Dominik Cinčić
Monday! 3
4
Tuesday! 5
o van translucent H O 3aa 3aa OH O H 3 C O Schiff O H 2 N H 2 N CH 3 CH 3 base blurry filtered OH H N translucent O CH 3 6
Crystallization Room temperature 96 % or absolute ethanol Crystallization 8 °C 96 % ethanol; very fast filtration of 3aa 96 % or absolute ethanol; slow filtration of 3aa 7
Crystallization Room temperature absolute ethanol; very fast filtration absolute ethanol ; very fast filtration of 3aa Crystallization 8 °C 8
Crystallization 8 °C 96 % ethanol; very fast filtration 9
Crystallization Room temperature 96 % or absolute ethanol; medium fast filtration 10
I rel. / a.u. III – 25 °c II – heated to 116 °C II – heated to 106 °C II – heated to 101°C II – heated to 82 °C II – at 25 °C 5 10 15 20 25 30 35 40 45 11 2 θ / °
12
13
Recommend
More recommend