Hydrochloric Acid → HCID 66939006, compound

Participants

Reaction Steps

Mix 1-methyl-4-(N-(2-fluoro-3-chlorophenyl)ethylamino)piperidine (Preparation 26) (0.367 g), benzophenone imine (0.295 g), Pd2(dba)3 (50 mg), 2-(di-t-butylphosphino)biphenyl (32 mg), and sodium t-butoxide (0.182 g) in toluene (10 mL) and heat at reflux for three days. Dilute with methanol (5 mL), 30 minutes after adding 2 mL of 5N HCl, load on a SCX column (10 g), wash with methanol, elute the product with 2M NH3 in methanol, evaporate and purify on a silica gel column (35 g), using a gradient of dichloromethane-2M NH3 in methanol to give 39 mg of the title compound: mass spectrum (electric spray) m/z=252 (M+1).

Provenance & Evidence