Water → HCID 20192464, compound

Participants

Reaction Steps

A solution of 6.76 g of crude 3-nitrosoperhydro-1H-pyrido[1,2-a]pyrazine (prepared according to stage (a)) in 30 ml of tetrahydrofuran is added dropwise at reflux temperature to a stirred suspension of 1.71 g of lithium aluminium hydride in 150 ml of tetrahydrofuran. The reaction mixture is stirred at room temperature for a further 3 hours; while cooling with ice 10 ml of aqueous 2N sodium hydroxide solution and then 10 ml of water are added and the whole is stirred at room temperature for a further 2 hours. The precipitate is filtered off with suction and then washed on the suction-filter with hot isopropyl alcohol. The filtrate (including the isopropyl alcohol portions) is concentrated by evaporation in vacuo and yields the desired 3-aminoperhydro-1H-pyrido[1,2-a]pyrazine (6.68 g) in the form of a slightly yellow-coloured oil of a purity that is sufficient for the hydrazone formation described above.

Provenance & Evidence