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Aldol condensation of phenanthrene-9-carboxaldehyde and acetone; (1E,4E)-1,5-Di(9-phenanthryl)-1,4-pentadien-3-one

SyntheticPage 774
DOI: 10.1039/SP774
Submitted Jan 28, 2015, published Jan 29, 2015
Matthew McBride (mcbridemj@gmail.com), Jean-Claude Bradley ()
A contribution from UsefulChem


			Reaction Scheme: <IMG src="/images/empty.gif">Aldol condensation of <SPAN id=csm1422618504790 class=csm-chemical-name title=phenanthrene-9-carboxaldehyde grpid="1">phenanthrene-9-carboxaldehyde</SPAN>&nbsp;and <SPAN id=csm1422618525576 class=csm-chemical-name title=acetone grpid="2">acetone</SPAN><IMG src="/images/empty.gif">

Chemicals Used

Phenanthrene-9-carboxaldehyde (Sigma Aldrich, 97%)
Acetone (Sigma Aldrich, 99%)
Sodium Hydroxide (NaOH)
Methanol 

Procedure

A solution of acetone (0.0171 g, 0.29 mmol, 1.0 eq) in methanol (1 mL) at room temperature was added to a stirred solution of phenanthrene-9-carboxaldehyde (0.154 g, 0.75 mmol, 2.5 eq) in methanol (45 mL). NaOH (0.9996 g, 25.00 mmol, 84.8 eq) was dissolved into the reaction mixture. The reaction mixture was stirred at room temperature for 72 hours. The precipitated product was recovered by suction filtration, washed 1x with 2-3mL of water and washed 1x with 2-3mL of methanol, and dried over suction. The crude product was recrystallized in benzene, cooled to room temperature, washed 1x with 2-3mL of benzene, dried over suction, and recovered (0.0242 g, 19%) as yellow crystals (mp 264-265°C).  

Author's Comments

•The product was insoluble in methanol allowing for recovery by filtration.
•A trace impurity of benzene was present in the final product as determined by the NMR spectrum.   

Data

1H NMR Spectrum (500 MHz, CDCl3): δ 8.78 (d, 2H), δ 8.72 (d, 2H), δ 8.68 (d, J = 16.5 Hz, 2H), δ 8.33 (d, 2H), δ 8.16 (s, 2H), δ 7.98 (d, 2H), δ 7.69 (m, 8H), δ 7.36 (d, J = 15.5 Hz, 2H) 



Lead Reference

M. J. McBride, J. C. Bradley. UsefulChem, Experiment 286. http://usefulchem.wikispaces.com/EXP286

Supplementary Information

1H NMR Spectrum

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Keywords: Aldol Condensation