Sodium Hydroxide → HCID 20283107, compound

Participants

Reaction Steps

To a suspension of 4.68 g of lithium aluminum hydride (61.7 mmol, 50% in oil; washed 3 times with hexane) in 160 ml of THF was added dropwise a solution of 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-(4-chlorophenoxy)piperidine (liberated from 34.7 g, 0.105 mol, of the oxalate) in 160 ml of dry THF. The mixture was stirred at reflux for 16 hours, allowed to cool to room temperature and subsequently cooled in an ice bath. To the mixture were added slowly, dropwise, 3 ml of water, 3 ml of 15% NaOH and 9 of ml water. The mixture was filtered and the residue washed with THF. Evaporation of the solvent provided an oil. The oil was washed with water, dried over potassium carbonate and the solvent evaporated to provide an oil. The yield of the dihydrochloride was 11.98 g (63%).

Provenance & Evidence