Hydrochloric Acid → HCID 178441516, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of methyl 4-[N-(2'-cyanobiphenyl-4-yl)methyl-N-valerylamino]-3-nitrobenzoate (1.7 g), sodium azide (3.9 g) and ammonium chloride (3.2 g) in DMF (17 ml) was stirred at 115 ° C. for 5 days. To the reaction mixture was added water and the mixture was neutralized with 1N-HCl, followed by extraction with ethyl acetate. The organic layer was washed with water, dried and concentrated to dryness. The concentrate was purified by column chromatography on silica gel to give crude crystals. Recrystallization from ethyl acetate gave colorless needles (0.67 g, 34%), m.p. 134-136° C.

Provenance & Evidence