Conditions: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: A mixture of isobutyl-(2-fluoro-phenyl)-ketone 13 (0.928 gm, 5 mmole), piperidine (0.645 gm, 7.82 mole) and potassium carbonate (1.08 gm, 7.82 mmole) in 4 ml of DMF was heated for 4 hrs at 120° C. After completion of the reaction (monitored by TLC), the reaction mixture was cooled and water (30 ml) was added to the reaction mixture and then extracted with ethyl acetate (1×15 ml, 2×7 ml). The combined organic layers were washed with a saturated ammonium chloride solution (2×15 ml) and subsequently dried over sodium sulphate. The solvent was removed under reduced pressure to obtain isobutyl-(2-piperidino-phenyl)-ketone 10 in 95% yield (GC showed 90% Purity). 1HNMR CDCl3, (spectrum 13): 0.92(d, 6H), 1.60(m, 6H), 2.07(m, 1H), 2.95(m, 6H), 7.05(m, 2H). 7.35(m, 2H). IR (spectrum 14) (Neat): 2841, 1657(C═O), 1570, 1435, 1345, 738
After completion of the reaction (monitored by TLC)
the reaction mixture was cooled
extracted with ethyl acetate (1×15 ml, 2×7 ml)
The combined organic layers were washed with a saturated ammonium chloride solution (2×15 ml)
subsequently dried over sodium sulphate
The solvent was removed under reduced pressure
Source ID: ord-0190ea449e9044a8b9fe895b031163a3