1,4,7,10-Tetraazacyclododecane → HCID 18471400, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 0.52 g of 1,4,7,10-tetraazacyclododecane, 0.32 g of tetraazacyclododecane tetrahydrochloride, 0.77 g of ethyl orthocarbonate, and 5 ml of absolute ethyl alcohol was heated with stirring on a steam bath (ca. 100°C) for 8 hours. The nmr spectrum of a small sample of the mixture indicated that the desired reaction was about 75-80% complete. The mixture was heated with stirring on a steam bath for 19 hours more. Volatile materials were evaporated under reduced pressure, and the residue was recrystallized from acetonitrile to give 0.20 g of 1,2,3,4,6,7,8,9-octahydro-5H-4a-azonia-2a,7,9a-triazacycloocta[cd]pentalene chloride (II) as needle-like crystals.

Provenance & Evidence