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- This is the text of Purity's
computer file document,
lab2.txt, the last chemistry lab write up she completed
with lab partner Kevin Stark.
- -----------------------------------------------------------
- Fundamentals of Organic Chemistry
- Chemistry 223 - Section 4: Coulter Hall Lab
- Unit: Aldehydes and Ketones
- Ariadne P. Knight & Kevin T. Stark
- February 14, 1997
-
- Aldol Condensations on Supported Reagents
-
- Equipment:
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- 8 mL SPE reservoir with frit
- stopcock
- reservoir support and bracket
- beaker
- cut tip transfer pipet
- 1 mL calibrated transfer pipet
- test tube
- microliter syringe
- safety equipment, goggles, gloves
- MSDS sheets
-
- Purpose:
-
- Analyze the solution to determine the percent
conversion of reactant to product, and isolate and purify
product. Accomplish condensations using SPE tubes and
ion-exchange resins for Chalcone, Dibenzalaceton,
Monobenzalacetone.
-
- Procedures:
-
- Step 1. Fit 8 mL SPE reservoir with closed stopcock
and support. Ensure frit pressed evenly in bottom.
- Step 2. Wash basic anion exchange resin, Amberlite
IRA-400 (OH) in 0.5 mmol each of benzaldehyde and
acetophenone by creating a slurry of resin in the
solvent.
- Step 3. Add 2 mL of resin to resevoir using cut tip
transfer pipet.
- Step 4. Allow resin to settle.
- Step 5. Once resin has settled, the stopcock is
opened and solvent allowed to drain from the reservoir.
- Step 6. Mix reagents to be used in a test tube with
0.5 mL solvent to solution and transfer to top of resin
bed in reservoir with poly transfer pipet. Wash test tube
with another 0.5mL solvent and add to reservoir.
- Step 7. As necessary, add solvent until 1 to 2 mm
above the top of the resin bed ensuring that the reaction
solution is in contact with the entire resin bed.
- Step 8. Agitate gently to to mix reagent solution.
Using a 1 mL calibrated poly transfer pipet, insert to
bottom of resin bed and squeeze bulb slowly.
- Step 9. Allow solution to stand for 30 minutes. As
necessary for crystallization, add enough solvent to
dissolve product.
- Step 10. Open stopcock and allow the contents to
drain into flask. Wash resin with one bed-volume of
solvent.
- Step 11. Analyze the solution to detemine the percent
conversion of reactant to product, and isolate and purify
the product.
-
- Specific Procedures:
-
- 1. For Chalcone, use 0.5 mmol each of benzaldehyde
and acetophenone
- 2. For Dibenzalacetone, use 0.25 mmol of acetone and
0.50 mmol of benzaldehyde
- 3. For Monobenzalacetone, use 0.25 mmol of
benzaldehyde and 2.0 mmole of acetone
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- (Kevin's observations and our conclusions here, Kevin
thinks we should print out separately and just copy)
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