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Question: what is the overall reaction for this preparation of a racemic mixture of (+) and (-)[Co(en)3]3+? Procedure: Preparation of a racemic mixture of (+)
Question: what is the overall reaction for this preparation of a racemic mixture of (+) and (-)[Co(en)3]3+?
Procedure: Preparation of a racemic mixture of (+) and (-)[Co(en)3]3+ Add to a 400 mL beaker distilled water (15 mL) followed by ethylenediamine (6.2 g, 6.9mL). add 3 mL concentrated hydrochloric acid and a solution of 9.3 g CoSO47H2O in 20 mL water. Add 6.6 mL 30% H2O2 dropwise. The solution now contains a racemic mixture of [Co(en)3](SO4)Cl. Preparation of the resolving agent, barium (+)-tartrate: Dissolve 8.1 g BaCl22H2O in water (~ 15 - 20 mL) and heat the solution to 90o. Simultaneously, dissolve 7.8 g of potassium (+)-tartrate (or 9.4 g sodium potassium (+)-tartrate) in a minimum amount of water (about 12 mL). Mix the two solutions whilst they are still warm.Stir the solution well and cool in an ice bath. Vacuum filter and wash the precipitate of barium (+)-tartrate with warm water. Separation of the enantiomers: Pour 30 mL of DI water into100 mL beaker and put a mark on the beaker. Add all the solid barium (+)-tartrate prepared earlier to the solution of [Co(en)3]3+. On a hot plate warm the solution to 70o (do not boil!) stirring vigorously with a glass rod for about 15 minutes. While the solutionis still hot, vacuum filter the precipitated barium sulfate. Transfer the filtrate to a 100 mL beaker with the mark. Evaporate the filtrate (keep the temperature below 90o, do not boil!) to a volume of 30 mL. Do not go below this volume as this will cause the other isomer to start precipitating. Cool in an ice bath for 20-30 minutes scratching the sides of the beaker with a glass rod. Consult with your instructor if no precipitate forms after 30 minutes. Vacuum filter the crystals of [(+)- Co(en)3][(+)-tart]Cl5H2O. Prepare a solution of 20 mL 95% ethanol and 30 mL water. Use this to wash the crystals. Cleavage of the resolving agent: Redissolve the crystals in 10 mL hot water (~60o) and add one drop of concentrated ammonia solution. Stir and add a solution of 11.3 g sodium iodide dissolved in 5 mL hot water. After cooling in an ice bath, vacuum filter and wash the crystals with first a little ethanol and then a little acetone. Record the yield of [(+)-Co(en)3]I3H2O, and hand in the remaining material in a labelled vial to be retained for next week.
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