Manufacturing Process
Conc. sulfuric acid (11 ml) was added to 4-(N,N-dimethylamino)-2-phenyl-2-
(2-pyridyl)-valeronitrile (6.3 g) at 0°C. Then water (1 ml) was added thereto.
After being heated at 90°C for 3 hours, the mixture was poured into ice-water,
adjusted to pH 10 with 10% aqueous sodium hydroxide and extracted with
ethyl acetate (3x50ml). The extracts were combined, and washed with water,
dried over magnesium sulfate and evaporated under reduced pressure. The
obtained crude crystal was recrystallized from diethyl ether to give 4-(N,N_x0002_dimethylamino)-2-phenyl-2-(2-pyridyl)-valeramide (1.89 g). MP: 132-134°C.
Recrystallization from 40% water ethanol gave MP: 156-157°C. The structure
of the product was confirmed by UR, NMR (CDCl3) spectra and elemental
analysis.
