Monday, May 23, 2011

4th day (Friday)

waited until 3pm (reaction started on 12 pm on wednesday) because 12 pm is lunch time until 2.40pm.

(helped the others with their stuff while preparing my apparatus too)

Liquid was an amber brown colour with trace amount of white solids

Liquid was washed with squirts of cold water from the dropper and acid HCL (10%) (a few squirts too, more white solids were formed) was added to stop the reaction (by reacting with KOH).

Chloroform was added to dissolve the organic product, and separate the organic product from the aqueous solution.

Mixture was poured into separating funnel, aqueous layer was above and and organic layer was below (because chloroform is more denser than water). Organic layer was separated from aqueous layer into a conical flask. Aqueous layer was washed with chloroform (because some products could be trapped in the aqueous layer) and the chloroform was added into the organic layer. Organic layer was cloudy, meaning there's still water in the organic mixture. Brine (supersaturated NaCl solution) was added into the organic layer to extract water, and water was eliminated by adding MgSO4.

Mixture was filtered to remove MgSO4, and then the next process was to conduct a simple TLC.

Conducting TLC.

Purpose of conducting TLC is to determine if any reaction occured to your reactants and to see if there are any products.

3 things were prepared:
a little bit of solid reactant 1 was dissolved in chloroform in a small vial.
Same thing for solid reactant 2.
A glass jar was added 4ml petroleumn ether and 1 ml ethyl acetate lefta while fior the mixture vapour to fill the jar.
4 spots were spotted on a piece of silica paper (4cmx5cm), R1, R2, P1 and P2 (2 spots of product, just to be safe) and placed vertically into jar.

Waited for solvent to soak the paper approx 90%, , paper taken out, dried, put under shortwave light.

Spots were circled, and analyzed.

The 2 spots on both P1 and P2 corrolated with the spots on R1 and R2, meaning there was NO REACTION TO GIVE PRODUCT.

T_T


My two and half days wasted, thank you very much claisen-schmidt condensation!









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