Dichloromethane → HCID 13556894, compound

Participants

Reaction Steps

A mixture of 40 ml of 98% diethylamine, 50 ml of methylene chloride, 0.6 g (0.9 mmole) dichlorobis(triphenylphosphine)palladium (II), 0.15 g (0.8 mmole) cuprous iodide, 3.8 g (10.8 mmole) of 8-chloro-5-bromo-1-(2-fluorophenyl)-3H-2-benzazepine and 3 g (16 mmole) of propargyl phthalimide was stirred under nitrogen at room temperature for 24 hr. The mixture was concentrated at reduced pressure to dryness. The residue was dissolved in methylene chloride and washed with water. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to dryness. Purification of the residue by column chromatography (silica gel, 50 g; eluent, methylene chloride gradient to 5% ether in methylene chloride) gave as the major fraction a colorless solid. Recrystallization from ether gave colorless needles, mp 164°-165° C.

Provenance & Evidence