Sciencemadness Discussion Board

how to synthesis the tris-betaalaninatocobalt(iii)

ahlok2002 - 11-2-2004 at 04:41

i need help!
i actuatly involve in some syudy in the synthesis of thecobalt(iii) complexes of amino acids.
i want to synyhesis the tris-betaalaninato cobalt(iii), but the product not succesful then i need some help.
now i'm going to show you all the ways i make the complex then in between if you all got any suggestion please point out!

first, i synthesis the hexaaminecobalt(iii) chloride from the CoCl2.
5.0g CoCl2.H2O+3.3gNH4Cl to 30ml of distilled water.
then add 1.0g of activated chacoal and 45ml con.aqueous ammonia.
cool the brown slurry in the ice bath to 0'C then add 4ml of 30% H2O2. the broen mixture ias incubate for one hour at 60'C.
afther that cool the mixture to 0'C and product precipitate from the solution with charcoal, collect the product and the charcoal by filtration. (the filtrate I is collected and con HCl is added the the darker orange solid is collected.) the residues undergo recrystallization to seperate the product from the activated charcoal by adding 40ml water and 1ml con HCl,heat to 70'C. collect the filtrate II and add the cold con HCl then the orange solid is collected.
i run the IR for both darker orange and orange solid, yet give me the same pick at most of the picks except the two weak picks at 1377.7 and 1354.9/cm.

so the question is whether this two compounds are the same [Co(NH3)6]Cl3 or in isomers?

i continue the experiment by assume that all the orange solid are [Co(NH3)6]Cl3.
so i mixed ,
[Co(NH3)6]Cl3 +3 (beta aniline) + 3KOH in round flask with air condenser,the whole is heat to 100'C( reflusk ) until some crytaline appeared in it ( 2-3 hours) suppose to get the violet crystal afther colling. yet i get the black solid out in the residue and dark red filtrate!

so i don't know which step is wrong whether the tmperature is to high or reflusk too long until decomposed?

please give some guide or better preparatio ways.or got web page relevant to the synthesis welcome reply me.