Organic Planning Flashcards
Apparatus req
Heating mantle
Round bottom flask
Liebig condenser
Clamps
Flow of water?
| -> out | | ->in| |
Procedures for rn
Weight accurately X g of -RCOOH in a DRY around bottom flask in a weighting balance;
Clamp in cold water;
Y cm3 of B from a dropping funnel, DROP BY DROP into the contents of the round-bottom flask w constant stirring;
8-9 drops of catalyst;
Replace cold water bath w heating mantle; attach a liebag condenser on top of the round bottom flask;
Slowly increase the power of heating mantle; bring the rn mixture to a gentle boil; reflux mixture for 15 mins;
After 15mins, switch off heating mantle; allow condensate in condenser to drain back into flask; content cook back to rtp;
Remove heating mantle and replace with cold bath;
Add 2-3cm3 of H2O drop by drop into round bottom flask using a dropper; content cool back to rtp
Pour content into abt 50 cm3 of cold water in a 250cm3 beaker
Describe purification
Filter the mixture;
Wash (s) on filter paper once w H2O;
Make a hole on filter paper w glass rod, wash down all (s) w hot ethanol into a clean 100cm3 conical flask;
Dissolve the solid using a min amt of hot ethanol;
Filter the hot solution into another clean 100cm3 conical flask;
Add hot water slowly to the sol until (s) separate out; warm the mixture until a clear sol is obtained again;
Cool the sol to obtain the crystallized solid;
Filter the recrystallized (s), wash w H2O;
dry the (s) by pressing it under several layers of filter paper;
Measure MP; check purity of aspirin obtained