Potassium Iodide → HCID 21968276, compound

Participants

Reaction Steps

A mixture of 3-(2-chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (2.45 g), disclosed in EP-0,196,132, intermediate 5 (2.7 g), sodium carbonate (3.3 g) and potassium iodide (0.1 g) in methyl isobutyl ketone (250 ml) was stirred and refluxed for 18 hours. The reaction mixture was cooled, filtered and the filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent: CHCl3 /CH3OH 90/10). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from ACN (25 ml). The crystals were filtered off and dried, yielding 2.3 g (50%) of (±)-cis-3-[2-[1,3,4,4a,5,9b-hexahydro-5-(phenylmethyl)-2H-pyrido[4,3-b]indol-2-yl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (compound 9, mp. 145.1° C.).

Provenance & Evidence