Aluminium lithium hydride → HCID 12290108, compound

Participants

Reaction Conditions

Reaction Steps

11-Hydroxy-11-methyl-5,11-dihydro-dibenzo[b,e]azepin-6-one (3) (51.6 g 0.22 mol) was added to a suspension of LiAlH4 (33 g, 0.88 mol) in dioxane (850 mL). The reaction mixture was heated to 105° C. After 2.5 h under reflux the reaction mixture was cooled, the excess LiAlH4 was destroyed with aqueous Na2SO4 (55 mL). ethyl acetate (1.81) and Na2SO4 (440 g) were added, the reaction mixture was stirred for 30 min. The solids were filtered off and the filtrate was concentrated under reduced pressure. The crude product was purified by column chromatography on silica (Heptane:Ethyl acetate=6:4) to give 6,11-dihydro-11-methyl-5H-dibenzo[b,e]azepine (4) (28 g, 61%) Data: (m/z)=210 (M+H)+.

Provenance & Evidence