Hydroxylamine → HCID 54212349, compound

Participants

Reaction Steps

NaOCH3 (0.189 mol; 30% in CH3OH) was added to a solution of hydroxylamine (0.189 mol) in ethanol (105 ml) The mixture was stirred at RT for 15 minutes and then filtered. The filtrate was added to a mixture of 2-chloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2-(3H)-yl)benzeneacetonitrile (0.054 mol) in ethanol (55 ml). The mixture was stirred at 60° C. for 1 hour, stirred and refluxed for 2 hours and stirred at RT overnight. The solvent was evaporated. The residue was taken up in water and extracted with EtOAc. The organic layer was separated, dried, filtered and the solvent was evaporated, yielding 20.3 g of (±)-2-chloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)-N′-hydroxybenzeneethanimidamide (interm. 66).

Provenance & Evidence