Water → HCID 15956290, compound

Participants

Reaction Steps

A solution of 5,11-dihydro-11-ethyl-5-methyl-2-(3-pyrrolyl)-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.093 g) in DMF (1 mL) and CH3CN (1 mL) was cooled to -50° C., and chlorosulfonyl isocyanate (0.041 g) was added in one portion. The resulting mixture was allowed to warm to room temperature and stirred for 2 h, then poured into water, extracted with CH2 Cl2, dried (anhyd Na2SO4), filtered, and evaporated. The residue was purified by preparative plate chromatography (ether) to give two pure compounds. Crystallization of each of these pure compounds from ethyl acetate/pet ether provided 0.038 g of the title compound, mp 262°-263° C., and 0.038 g of 2-(2-cyanopyrrol-4-yl)-5,11-dihydro-11-ethyl-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, mp 268°-269° C.

Provenance & Evidence