Piperidone Synthesis

and methyl iodide(5ml) were added to the solution. The mixture was heated on a water bath for three hours. Acetone was removed and the residue was poured into water()150ml. The solid N-methypiperidone separated was filtered and recrystallised from ethanol.
4.6.General procedure for Preparation of the N-methylation of piperidin-4-one oximes: The piperidone (0.1mol)was dissolved in ethanol(50ml). saturated solutions of hydroxylamine hydrochloride and sodium acetate in water were added. The mixture was refluxed on a water bath for one hour. Then it was cooled , poured into water and the solidoxime obtained was filtered. All the oximes were recrystallised from ethanol.
S.
No. KETONE m.pt.0C
1 1-Methyl -2,6- diphenylpiperidin-4-one 148 -149
sec-1 Sd. = 2.9 X 10 -3

Run – 3
Effect of oxidant
[ NMPO] = 1.00 X 10-2 M [ AcOH ] = 100 %
[PCC] = 1.127 X 10-3 M Temperature = 35 0 c

Time
Secs. Titre ml Log titre 270 5.4 0.7324
570 4.8 0.6812
900 4.3 0.6335
1205 3.8 0.5798
1465 3.5 0.5440
1640 3.2 0.5051
1885 2.9 0.4698

r = 0.999 k = 3.58 X 10-4 . sec-1 Sd. = 2.19 X 10 -3

Run – 4
Effect of oxidant
[ NMPO] = 1.00 X 10-2 M [ AcOH ] = 100 %
[PCC] = 1.353 X 10-3 M Temperature = 35 0 c

Time
Secs. Titre ml Log titre 270 5.4 0.7324
570 4.8 0.6812
900 4.3 0.6335
1205 3.8 0.5798
1465 3.5 0.5440
1640 3.2 0.5051
1885 2.9 0.4698

r = 0.999 k = 3.44 X 10-4 . sec-1 Sd. = 4.08 X 10 -3

Run – 5 Effect of oxidant
[ NMPO] = 1.00 X 10-2 M [ AcOH ] = 100 %
[PCC] = 1.578 X 10-3 M Temperature = 35 0 c Time
Secs. Titre ml log