Sodium borohydride → HCID 69022176, compound

Participants

Reaction Steps

Sodium tetrahydroborate (2.68 g) was added portionwise at 5° C. to a solution of intermediate (27) (0.0354 mol) in methanol (150 ml). The solution was poured into ice water and extracted with DCM. The organic layer was dried (MgSO4), filtered off and evaporated. The residue (12.27 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 97/3/0.1). The pure fractions were collected and evaporated. The residue was crystallized from methanol, yielding 10.4 g (78%) of (±)-7-[(4-chlorophenyl)hydroxymethyl]-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (intermediate 28).

Provenance & Evidence