Aluminium lithium hydride → HCID 14390915, compound

Participants

Reaction Steps

To lithium aluminum hydride (21 g) in ether (150 ml) was added 1,2-dibenzoyl-5-[4,4-bis(4-fluorophenyl)butyl]hexahydro-1H-1,2,5-triazepine hydrochloride (34.4 g) slowly in small portions. The mixture was stirred and heated under reflux with protection from moisture for 22 hours. The reaction was quenched with 10% sodium hydroxide and water. The resulting hydroxides were collected on a filter and washed well with ether. The filtrate and washings were evaporated to a syrup, wt. 30.4 g. The syrup was dissolved in acetone and the solution was decolorized (Nuchar). The solution was concentrated and a solution of fumaric acid (6.7 g) in acetone (800 ml) was added. The resulting solution was boiled down until crystallization occurred. After cooling, the crude product was collected on a filter and washed with acetone; wt. 32.9 g. Recrystallization from methanol-ether gave 25.3 g (68%) of pure titled product as the fumarate salt (1:1), mp=184°-185°.

Provenance & Evidence