Butylamine → HCID 19063101, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 4 g of the compound prepared in Example 18 and 30 ml of n-butylamine in 10 ml DMSO is warmed at 140° C. for 20 h in a closed flask. The solution is evaporated under vacuum, the oily residue is treated with 200 ml H2O and extracted with CHCl3 (3×50 ml). The vitrous residue, obtained by evaporating the organic phase, is dissolved in 40 ml EtOH 95%, the solution is added with 10 ml KOH 0.3N and warmed to reflux for 30'. The residue obtained by evaporation of the solution is purified by flash chromatography on SiO2 column eluting with a CHCl3 /MeOH gradient from 100:3 to 100:10. The crude product, obtained by evaporating the fractions containing the pure compound, is dissolved in 75 ml EtOH, the solution acidified with HCl in EtOH 4N and the hydrochloride is collected by filtration, crystallized from EtOH 90% giving 2.5 g (53%) of the wanted compound; m.p.: 260°-262° C.

Provenance & Evidence