Hydrochloric Acid → HCID 15586694, compound

Participants

Reaction Steps

A solution of 7.0 g (0.017 mole) of 2-chloro-N-[2-[[3-(dimethylamino)propyl]phenylamino]-3-pyridinyl]benzamide and 10.5 g (0.069 mole) of phosphorus oxychloride in 5 ml of 1,1,2,2-tetrachlorethane was heated under nitrogen atmosphere at 110°-115° C. for 16 hr. The cooled reaction mixture was poured into ice and 10 ml of dilute hydrochloric acid added. The mixture was extracted twice with petroleum ether. The acidic portion was made basic with sodium hydroxide pellets and thereafter extracted twice with methylene chloride. The combined methylene chloride extracts were washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was crystallized from isopropyl ether yielding 6.0 g (90%) of material. Recrystallization from isopropyl alcohol-isopropyl ether gave a yellow solid, m.p. 104°-105.6° C.

Provenance & Evidence